Construction and Building Materials 324 (2022) 126531

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Construction and Building Materials

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

Performance of waste glass powder as a pozzolanic material in blended

cement mortar
Qiong Li a, Hongxia Qiao a, b, *, Aoyang Li a, Guanjun Li c
a
School of Civil Engineering, Lanzhou University of Technology, Lanzhou, Gansu, China
b
Key Laboratory of Disaster Prevention and Mitigation in Civil Engineering of Gansu Province, Lanzhou University of Technology, Lanzhou, China
c
China Construction First Group the Fifth Construction Co. Ltd, Beijing, China

A R T I C L E I N F O A B S T R A C T

Keywords: In this study, the pozzolanic activity of finely ground waste glass powder (WGP) used as a partial cement
Blended mortar replacement in mortars was investigated, and the WGP particle size, WGP content, and curing age were selected
Waste glass powder for analysis. Tests to determine the fluidity, compressive strength, scanning electron microscopy (SEM), energy
Mechanical properties
dispersive X–ray spectroscopy (EDS), X–ray diffraction (XRD), Thermo–gravimetry analysis (TGA), Differential
Microstructure
Mass loss
thermal gravity (DTG) and Fourier transform infrared spectroscopy (FTIR) were performed on a blended mortar.
The results showed that when the WGP particle size was 20–44 μm and the WGP content was 20%, the fluidity of
the slurry was higher than that of the control group, and the slurry exhibits good cohesion and water retention
performance. When the WGP particle size ranges were 74–150 μm and 44–74 μm, the compressive strength of the
blended mortar was smaller than that of the control group for all curing days regardless of the WGP content.
When the WGP particle size was 20–44 μm, the compressive strength was lower than that of the control group at
7 d of curing, whereas it was 3.5% and 9.6% higher than that of the control group at 28 d and 90 d curing,
respectively, with a WGP content 20%. When the WGP particle size was 15–20 μm, the compressive strength did
not significantly increase compared with when the WGP particle size was 20–44 μm for the same WGP content,
but slightly decreased. SEM and EDS showed that when the WGP particle size was 20–44 µm and the WGP
content was 20%, the hydration products in the microstructure of the cement slurry were abundant, whereas
pore cracks were few. This was additionally confirmed by XRD and TGA–DTG results, thereby verifying the
formation of the lowest content of calcium hydroxide (CH) and the highest content of calcium silicate gel in the
blended mortar. Variations in the Si–O and Al–O bond intensities shown in the FTIR spectrum supported this
conclusion. Furthermore, the TGA–DTG results showed that the increase in calcium silicate gel content from 28
d to 90 d was higher than that from 7 d to 28 d, and that the activity of the WGP was more significant in the later
curing period.

1. Introduction
According to annual estimations by the United Nations, waste glass
(WG) constitutes 7% of the global solid waste treatment, and plain glass
accounts for the largest proportion. These non-biodegradable glass
wastes not only occupy numerous landfills and cause severe land and
environmental problems, but also consume a significant content of en­
ergy and discharge high content of CO2 [1–2]. Using WG to process and
synthesize building materials instead of using cement or aggregates for
preparing concrete can effectively increase the recovery rate [3].
However, previous studies indicated that WG containing the
significant content of alkali and active SiO2 was prone to alkali-silicon
reactions (ASR), which form alkali-silicic acid gel (Na(K)–Si–H(gel));
consequently, concrete cracking and destruction occurs, thereby dete­
riorating structural safety [4–5]. Conversely, some studies indicated that
grinding WG to a certain fineness could effectively avoid harmful
expansion caused by ASR, and the characteristics of waste glass powder
(WGP) such as multi-angular surface, volcanic ash activity, and micro-
aggregate effect be manipulated to improve the strength and dura­
bility of concrete [6–7].
Scholars have qualitatively described the particle size and pozzolan
activity of WGP [8–10]. Jain et␣al. [11] reported that when the WGP

* Corresponding author at: School of Civil Engineering, Lanzhou University of Technology, Lanzhou, Gansu, China.
E-mail address: qiaohongxia@lut.edu.cn (H. Qiao).

https://doi.org/10.1016/j.conbuildmat.2022.126531
Received 7 October 2021; Received in revised form 4 January 2022; Accepted 18 January 2022
Available online 15 February 2022
0950-0618/© 2022 Elsevier Ltd. All rights reserved.
Q. Li et al. Construction and Building Materials 324 (2022) 126531

Fig.␣1. Morphology and SEM of WGP with different particle sizes.

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Q. Li et al. Construction and Building Materials 324 (2022) 126531

glass powder content exceeds 20% owing to the agglomeration of glass

particles. However, Wang et␣al. [19] did not observe any significant
changes in the compressive strength when cement was replaced by 25%
WGP, as compared with the control specimen. The authors also revealed
that owing to the formation of secondary calcium silicate (C–S–H) by the
pozzolash reaction, the mortar containing WGP exhibited a relatively

Table␣2
Properties of cement.
Setting time (min) Compressive strength Flexural strength
(MPa) (MPa)

Initial setting Final setting 3d 28d 3d 28d

120 225 22.3 45.4 6.2 8.4

Fig.␣2. XRD spectra of WGP.

particle size was less than 600 μm, the volcanic ash activity and filling
effect were better; consequently, the porosity of concrete reduced, and
acid and salt erosion resistance improved. Idir et␣al. [12] investigated
the pozzolanic activity of blended glass with particle size ranging from
40 μm to 2.5 mm and concluded that the pozzolanic activity and
compressive strength increased as the particle size of WGP decreased;
subsequently, 40 μm was regarded as the critical value of pozzolanic
activity. Shao et␣al. [13] discovered that concrete containing 30%
cement replacement with a WGP particles size of 38 μm indicated 14.3%
and 33.3% higher compressive strengths than the concretes containing
WGPs measuring 75 and 150 μm, respectively. Mirzahosseini et␣al. [14]
investigated the effects of three green cullet sizes, i.e., 63–75, 25–38,
and 0–25 μm, on the reactivity of glassy auxiliary cementitious materials
and concluded that the content of calcium hydroxide (CH) in the Fig.␣3. Particle size distribution curve of sand.
cementitious materials with particle measuring 0–25 μm decreased
significantly at 7 d of curing. The high activity of volcanic ash was
attributed to the much higher surface area of 0–25 μm particles Table␣3
compared with that of other size ranges. However, Matos et␣al. [15] Mix proportion of blended mortar.
discovered that when the average particle size of WGP was similar to Specimen WGP WGP Cement WGP Fine Water
that of cement, the compressive strength was 3.5% lower, and the (M-A-B)* particle content aggregate
3
sizes (μm) (%) (kg/m )
flexural strength was 6.25% higher when 20% of cement in mortar was
replaced with WGP, as compared with the control specimen. In sum­ M-C / 0 450 0 1350 225
mary, it could be concluded that the compressive strength and tensile M-I-10 74–150 10 405 45 1350 225
strength of concrete and mortar increased with the decrease of particle M-I-15 15 382 68 1350 225
size of WGP. However, owing to the diversification of WGP production M-I-20 20 360 90 1350 225
M-I-25 25 338 112 1350 225
sources and production methods, the conclusions were diverse.
M-II-10 44–74 10 405 45 1350 225
In addition to the effect of the particle size of WGP on the activity of M-II-15 15 382 68 1350 225
pozzolana reaction, the WGP content is vital to the strength develop­ M-II-20 20 360 90 1350 225
ment of blended mortar and concrete. Jang et␣al. [16] used 3%, 5%, and M-II-25 25 338 112 1350 225
M-III-10 20–44 10 405 45 1350 225
10% WGP instead of cement to prepare mortar, and it was discovered
M-III-15 15 382 68 1350 225
that the compressive strength of blended mortar containing 10% WGP M-III-20 20 360 90 1350 225
was higher than that of the control specimen. Ramakrishnan et␣al. [17] M-III-25 25 338 112 1350 225
used WGP (replacement rate 5–45%, interval 5%) as a cement substitute M-IV-10 15–20 10 405 45 1350 225
and the results showed that compared with the control group, the M-IV-15 15 382 68 1350 225
M-IV-20 20 360 90 1350 225
compressive strength, flexural strength, split tensile strength, and bond
M-IV-25 25 338 112 1350 225
strength increased by 44.2%, 6.31%, 9%, and 31.9%, respectively, at 28
*
d. A similar conclusion was reported by Aliabdo et␣al. [18]. The authors :No. M-C indicates control specimen; M-A-B, A indicates WGP particle sizes,
indicated that strength development might be adversely affected if the and B indicates WGP content.

Table␣1
Chemical composition of cementitious materials (wt%).
Materials SiO2 Al2O3 Fe2O3 CaO Na2O K2 O SO3 MgO

WGP 69.31 3.42 0.31 9.53 11.42 0.06 0.02 2.53

Cement 25.72 7.14 4.25 55.370 0.41 0.83 2.17 1.26

3
Q. Li et al.
Fig.␣4. Fluidity of blended mortar with different WGP content and parti­
cle sizes.
dense microstructure with fewer pores.
Curing age also significantly affects the strength development of
blended mortar or concrete. Idir et␣al. [12] discovered that the
compressive strength of a 30% WGP-blended mortar was lower than that
of control specimen until 90 d of curing. However, at 210 d, the
compressive strength was approximately 4% higher than that of the
control specimen. Sadiqulislam et␣al. [20] demonstrated that all con­
crete containing WGP (replacement rate 0–20%, interval 5%) exhibited
excellent mechanical properties compared with the control specimen at
Fig.␣5. Compressive strengths of mortars with different WGP particle sizes.
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Construction and Building Materials 324 (2022) 126531
365 d; it was reported that the mechanical properties of concrete with
20% WGP was approximately 22.1% higher than that of the control
specimens. Kamali et␣al. [21] concluded that the strength of blended
mortar containing WGP increased significantly during 90 d to 365 d of
curing.
In previous studies, the effect of pozzolanic activity of WGP on hy­
dration products and microstructure was investigated via microscopic
analysis [22–25]. To ensure a pozzolanic reaction, the WGP for replac­
ing a portion of cement must contains a significant content of amor­
phous silica and a small content of Al2O3, such that CH was consumed in
the hydration products and additional C–S–H were created. Mirza­
hosseini [26] indicated that the hydration degree of WGP increased
when the curing temperature increased and the particle size distribution
decreased, thereby resulting in more and denser C–S–H gel and a higher
compressive strength. In addition, Nassar [27] reported that WGP
formed a denser and less permeable microstructure, which could
significantly increase the long-age period strength.
In summary, using a specific range of WGP particle size and content
replace a portion of cement to prepare blended mortar or concrete af­
fords improvements in the mechanical properties. However, some pre­
vious analyses focused on the effect of a single factor on the properties of
mixed mortar, and the analysis of the influencing factors was not
comprehensive. In the present study, three factors, i.e., WGP particle
size, WGP content, and curing age, were selected to analyze the effect of
WGP on the mechanical properties of blended mortar. The microstruc­
ture of the mortar was analyzed using scanning electron microscopy
(SEM) coupled with energy dispersive X–ray spectroscopy (EDS). The
formation of various mineral compounds was indicated via X–ray
powder diffraction (XRD) patterns. Fourier transform infrared spec­
troscopy (FTIR) was performed to investigate the changes in different
Q. Li et al.
Fig.␣6. Compressive strengths of mortars with different WGP content.
functional groups or chemical bonds in the mortar specimens. Finally,
thermo–gravimetric analysis (TGA) and differential thermal gravity
(DTG) were performed to quantitatively calculate the content of CH,
CaCO3, and C–S–H. In this experiment, the pozzolanic activity of WGP is
investigated comprehensively from a macro and microscopic perspec­
tive, thereby providing a theoretical basis for improving the utilization
rate of WGP.
2. Experimental program
2.1. Materials
As plain and clear glass accounts for a large proportion in the waste
glass, the discarded clear glass was used for the study in this experiment.
To obtain clean glass waste pieces, glass factory scraps were recycled,
classified, cleaned, dried, and impurity removed. The SM–500 grinder
was used to grind the glass for different times and sieve the ground glass
to the desired particle size using 100, 200, 325, 625, and 800 sieves,
yielding four different classes: 74–150 μm (I), 44–74 μm (II), 20–44 μm
(III), 15–20 μm (IV). The specific surface were 242 m2/kg, 298 m2/kg,
430 m2/kg, and 462 m2/kg, respectively. The macro and micro mor­
phologies of the four particle sizes of WGP were shown in Fig.␣1. The
mineral composition of WGP was determined by XRD, as shown in Fig.
␣2. X–ray fluorescence analyzer (XRF) was used to determine the basic
chemical composition and content of WGP (see Table␣1).
Ordinary Portland cement with a grade of 42.5, based on Chinese
standard GB/T 175-2007 [28] and the properties were shown in Tables 1
and 2. The specific surface area of cement was 364 m2/kg. River sand
with a fineness modulus of 2.78 and an apparent density of 2540 kg/m3
was used as the fine aggregate, and the particle size distribution curve of
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Construction and Building Materials 324 (2022) 126531
fine aggregate was shown in Fig.␣3.
2.2. Mortar blended proportions and preparation
Four WGP particle sizes were used in this study: 74–150 μm (I),
44–74 μm (II), 20–44 μm (III), and 15–20 μm (IV). The WGP content
varied from 10%, 15%, 20%, and 25% by the mass substitution of
cement. In addition, to investigate the effect of curing age on the me­
chanical properties of blended mortar, curing ages of 7 d, 28 d, and 90
d were selected. The water-to-binder ratio was set as 0.5, and the mix
proportion of the blended mortar are presented in Table␣3.
The mix proportion of blended mortar, molding and curing of the
specimens based on the Chinese standard GB/T17671-1999 [29].
Seventeen groups of specimens (with a size of 40 × 40 × 160 mm) were
prepared 3 test pieces in each group, 51 in total. After preparation, the
specimens were set in the mold for 1 d and then demolded and cured in a
fog room (20 ◦ C ± 2 ◦ C, 95 % relative humidity) for 28 d.
2.3. Methodology
2.3.1. Fluidity test
The fluidity test of fresh cement mortar was in accordance with
Chinese standard GB/T2419-2005 [30]. The blended mortar was
divided into two layers into the mold (height 60 mm), with the tamping
bar from the edge to the center of uniform tamping 15 times for each
layer, and lift the mold vertically upwards. Start the jumping table and
complete 25 jumps in 25 s ± 1 s at a rate of one jump per second. Then
the caliper was used to measure the diameter of the two perpendicular
directions of the bottom surface of the mortar, and the average value
was calculated.
Q. Li et al.
Fig.␣7. Curved surface model fitting diagram of WGP particle sizes and WGP content against the strength.
2.3.2. Mechanical strength test
The compressive strength test was measured for mortar prisms with
the curing age of 7 d, 28 d, and 90 d in accordance with Chinese standard
GB/T17671-1999 [29]. Rate of loading was kept as 0.5 MPa/s with the
applied load perpendicular to the surface of specimen. Three test spec­
imens were prepared for each group, and the average value was
considered to be the strength of the group (the deviation between the
individual and average strengths should not exceed 15%).
2.3.3. Microscopic tests
A JSM-6701F cold field emission electron microscope was adopted to
perform SEM. The image resolution was 1 nm (15 kV), the magnification
was 25 × –650 000× times, and the acceleration voltage was 0.5–30 kV.
A small sample measuring approximately 10 mm × 10 mm was obtained
from each of the mortar specimens, placed in acetone (to prevent hy­
dration), and dried in an oven at 60 ◦ C for 24 h. A magnification of
5000× was used to image the sample. The EDS was used for element
analysis of samples. JSM-5600LV low vacuum scanning electron mi­
croscope X–ray spectrometer with resolution of 127 eV was used.
XRD was performed using a D8 ADVANCE X–ray powder diffrac­
tometer. The scanning speed was 2◦ /min, the step interval was 0.02◦ per
step, and the scanning angle was 5.0◦ – 65.0◦ . A small sample with a size
of 1 cm3 was obtained from each mortar specimen and placed in abso­
lute ethyl alcohol. Then, it was ground into a powder and passed
through 80 um sieves in order to remove sand that was mixed with it as
much as possible and reduce the influence of sand on the test results. The
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Construction and Building Materials 324 (2022) 126531
samples were then dried at 60 ◦ C for 24 h. The preparation process of the
FTIR and TGA test samples was the same as that for the XRD test.
The FTIR spectra were recorded using a NICOLET series spectro­
photometer. Spectral analysis was performed over the wavenumber
range of 2000–300 cm− 1, and the spectral resolution was set to
0.09 cm− 1. The specimens were prepared by blending 1 mg of the
sample in 300 mg of KBr. The ground powder and the dry KBr were
blended uniformly at a mass ratio of 1:100 and then loaded into an
abrasive tool. A SYP-24B tablet press was pressed into thin sheets
measuring 0.1–1 mm under a pressure of 20 MPa.
TGA was performed on the powdered samples using a
Q1000DSC + TGA instrument. The parameters involved were as follows:
test temperature range, room temperature (RT) to 900 ◦ C; heating rate,
10 ◦ C / min; atmosphere, N2; the test reference material, was Al2O3. In
the present study, the results obtained from TGA was used to estimate
the CH content in the blended mortar from the mass loss measurement.
The CH content was estimated using Eq.1 [31]:
MCH
CH(\%) = W) = WCH × (1)
MW
where WCH is the mass loss during dehydration of CH as percentage of
the ignited mass (%), MCH is the molar mass of CH (g/mol), MW is the
molar mass of water (g/mol).
Q. Li et al.
Fig.␣8. Correlation between tested value and predicted value of blended mortar compressive strength.
3. Results and discussion
3.1. Fluidity
Fig.␣4 presents a trend showing the effects of WGP particle size and
content on the fluidity of the mortar. Compared with the control group,
when the WGP content was 10%–25%, the fluidity of the mortar with
WGP I and WGP II was higher than that of the control group. The fluidity
of mortar containing WGP I and II with 25% content increased by 10.9%
and 7.4%, respectively, compared with the control group. However, a
significant content of slurry was observed around the fresh mixture,
resulting in the bleeding and inferior cohesion of the blended material.
This was attributed to the fact that when the WGP particle size was
larger than that of cement, the hydration rate of WGP was much lower
than that of cement in the initial stage of curing, which resulted in an
overall slowing down of the hydration rate of the system [32], increased
bleeding, weakened cohesion, and poor water retention; the greater the
WGP content, the more significant the negative impact.
The fluidity of the blended mortar with WGP III was higher than that
of the control group. The optimal WGP content was 20%, and the
fluidity was higher than that of the control group by 4.5%. At this time,
the slurry exhibited good cohesion, water retention, and no bleeding.
This was attributed to the low water absorption rate and smooth surface
of the WGP, which reduced the resistance of relative slip between the
cement particles and improved the fluidity of the slurry.
With an increased in the WGP IV content, the fluidity of the mortar
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Construction and Building Materials 324 (2022) 126531
decreased. Furthermore, the fluidity was lower than that of the control
group regardless of the WGP content, and the slurry was dry. This was
because the decreased in the WGP particle size increased the surface
area of particles with the same mass, which consequently increased the
amount of water required to hydrate the WGP and reduced fluidity.
3.2. Mechanical strength tests
3.2.1. Compressive strength
Fig.␣5 shows the compressive strength of blended mortar with
different WGP particle sizes at all curing ages. For different WGP con­
tent, the compressive strength first increased and then decreased as the
WGP particle size decreased. Based on 20% WGP content as an example,
the WGP particle size decreased from I to II, and the compressive
strength of the blended mortar at 28 d and 90 d increased by 10.9% and
15.6%, respectively. However, the particle size reduced from II to III,
and the compressive strength increased significantly by 46.9% and
57.4% at 28 d and 90 d, respectively. This indicates that the WGP was
low in activity when the WGP particle size exceeded 44 μm, and most of
the particles appeared in the cement mortar in the form of micro-
aggregates, which reduced the content of hydration products in the
system and decreased the strength.
The compressive strengths of the blended mortars with different
WGP content at different curing ages are presented in Fig.␣6. As shown
in Fig.␣6(a)–(b), in the mortars containing WGP I and II, their
compressive strengths at all curing ages were lower than that of the
Q. Li et al.
Fig.␣9. SEM images of blended mortar with different WGP particle sizes at the age of 28 days.
control specimen; in fact, the compressive strength decreased signifi­
cantly as the WGP content increased. This is attributed to the higher
content of WGP I and II with lower activity substituted for cement,
which reduced the content of hydration products produced and hence
the strength of the mixed mortar.
Fig.␣6(c) shows the different trends of compressive strength as the
content of WGP III increased at different curing ages. Although the
compressive strength of the mortar decreased as the content of WGP III
increased at 7d, the compressive strength of the mixed mortar increased
with the content of WGP III at 28 d and 90 d. Furthermore, the mortar
containing 20% WGP III exhibited the highest compressive strength
among all groups at 28 d and 90 d, which were in fact 3.5% and 9.6%
higher than the control specimen, respectively. Reference [22] also
obtained a similar conclusion, in that the incorporation of WGP
improved the strength at a later age. This may be attributed to the
pozzolanic property of WGP III, which resulted in a denser microstruc­
ture and improved the interfacial bonding between the fine aggregates
and cement paste in the blended mortars.
However, compared with the mortars containing WGP III, the
compressive strength of the mortar with WGP IV decreased at all curing
ages, as shown in Fig.␣6(d). This result does not mean that the smaller
the WGP particle size, the worse the performance of the pozzolanic. This
is because, besides its fineness, the glass powder’s water absorption will
also affect its strength to a certain extent. The water-binder ratio used in
this study was set as 0.5, and the WGP specific surface area was too
large, resulting in increased hygroscopicity and slurry consistency. As a
result, the mixing water that participated in cement hydration
decreased, which affected the content of the cement hydration product
CH. However, the reduction in CH content cannot fully stimulate the
active performance of WGP and will ultimately affect the number of
secondary hydration products of WGP. A slight decrease in intensity was
observed.
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Construction and Building Materials 324 (2022) 126531
3.2.2. Prediction model of mortar strength
According to the analysis in Section␣3.2.1, the WGP particle size,
WGP content, and compressive strength of the cube roughly conform to
quadratic functions, and the prediction model of mortar strength at
different curing ages was established as shown in Eq. (2):
fd = m1 + m2 φ + m3 η + m4 φ2 + m5 η2 + m6 ηφ (2)
where fd is the compressive strength of blended mortars (d = 7 d, 28 d,
90 d), φ is the WGP particle size (mm), η is the WGP content (%), m1 –m6
is the regression coefficient.
According to the experimental results, the nonlinear surface model
fitting diagrams of the WGP particle size and WGP content against the
compressive strength of blended mortars at curing days 7, 28, and 90
were prepared and are shown in Fig.␣7. The prediction equation for the
compressive strength of the blended mortar is shown in Eqs. (3)–(5):
f7 = 18.708 − 22.019φ + 102.529η + 327.270φ2 + 203.052η2 − 565.467ηφ
(3)
f28 = 35.931 − 157.724φ + 105.574η + 772.704φ2 − 260.014η2 − 523.583ηφ
(4)
f90 = 38.448 − 66.050φ + 78.264η + 532.484φ2 + 122.507η2 − 786.472ηφ
(5)
The predicted value of compressive strength was calculated accord­
ing to Eqs. (3)–(5), and the predicted and test value were compared, as
shown in Fig.␣8. The correlation coefficient R2 = 0.938 (7 d), R2 = 0.901
(28 d), R2 = 0.909 (90 d), respectively, indicating good correlation and
the optimum regression equation could predict mortar strength
perfectly.
Q. Li et al.
Fig.␣10. EDS images of blended mortar with different WGP particle sizes at the age of 28 days.
3.3. Microstructure of blended mortars
3.3.1. SEM analysis
The SEM images of the blended mortar containing 20% WGP with
different particle sizes at curing age of 28 d are shown in Fig.␣9. As the
WGP particle size decreased from I to III, the content of the hydration
products increased significantly, and a considerable amount of gels were
formed in the cement paste; moreover, the gels that formed were
embedded with each other. In the mortar sample containing WGP III,
almost no microcracks were observed (Fig.␣9(c)). However, Fig.␣9(d)
clearly shows that needle-shaped ettringite scattered inside the pores,
and a large amount of CH was embedded between the hydration prod­
ucts, indicating that the secondary hydration products of WGP IV were
less than those of WGP III.
At 28 days of curing, a large amount of CH is not consumed to
generate the C–S–H gel. From a microscopic perspective, a smaller WGP
particle size does not necessarily imply more hydration products. The
particle size of the WGP affects the hydration rate; however, the water
binder ratio is another important influencing factor. Furthermore, a
WGP particle with a smaller size would absorb more water, which would
negatively affect the hydration reaction. Therefore, the particle size of
WGP III was the best particle size in this experiment, which was
consistent its effect on the mechanical properties.
After the mixed mortar with different particle sizes of 20% was cured
for 28 days, EDS analysis was conducted, as shown in Fig.␣10. The red
area marked by SEM in Fig.␣9 is the test area. As the sample was treated
with gold spray before the test, the strongest peak in the graph was Au,
which was not marked in the graph because it was irrelevant to the
analysis in this study. It can be seen from Fig.␣10 that particle size has no
effect on the types of the main elements contained in the samples;
however, it has a greater impact on the element content. With a decrease
in the WGP particle size, the Ca/Si ratio gradually decreased, but when
9
Construction and Building Materials 324 (2022) 126531
the WGP particle size was IV, the Ca/Si ratio slightly increased. This is
because, for the same WGP content, when the WGP particle size was
larger, the secondary hydration reaction of the WGP was lower, and the
gel system was dominated by C–S–H gels generated by cement hydra­
tion, leading to a higher Ca/Si ratio in the overall gel system; when the
WGP particle size was small, WGP easily reacted strongly with CH in the
solution to generate a hydrated C–S–H gel, and more Si was consumed to
generate the C–S–H gel, leading to a decrease in the Ca/Si ratio in the gel
system.
The SEM images of the control specimen and the specimens with
different WGP III content at curing age of 28 d are shown in Fig.␣11.
Compared with the control specimen, the hydration products of the
blended mortar with 10% WGP were less abundant, and the internal
structure was relatively loose (Fig.␣11(a)–(b)). When the WGP III con­
tent was 15%, it was observed (see Fig.␣11(c)) that lamellar CH crystals
were arranged randomly and formed crystal clusters. However, the CH
crystal particles shielded the surface of fine aggregates, thereby result­
ing in inferior bonding with hydration products [33]. Fig.␣11(d) shows
that ettringite of hydration products of mortar with 20% WGP III
transformed from fine to coarse, as compared with control specimens,
and a monolithic amorphous C–S–H gel developed into a three-
dimensional C–S–H gel, which offers a higher strength [34]. Further­
more, the number of pores and cracks decreased, indicating that the
compactness of cement mortar improved, and the increase in the WGP
content promoted the hydration of cement. However, in the hydration
product of mortar with 25% WGP III (Fig.␣11(e)), the content of floc­
culated C–S–H gel increased significantly and contained pores that
exhibited a relatively loose structure. The SEM images show that the
cement slurry was the densest when the WGP content was 20%, which
macroscopically verifies that the compressive strength was the highest
when 20% WGP III was incorporated.
The SEM images of the specimens with a WGP III content of 20% at
Q. Li et al.
Fig.␣11. SEM images of blended mortar with different WGP III content.
curing ages of 7, 28 and 90 d are shown in Fig.␣12(a)–(c). Fig.␣12(a)
shows that, at the curing age of 7 days, the main hydration products in
the slurry were C–S–H gel, CH, and ettringite, and there were fewer
hydration products. Furthermore, holes and cracks were on the spec­
imen. Fig.␣12(b) shows that at a curing age of 28 d, the number of hy­
dration products increased significantly, the three-dimensional C–S–H
gel, lamellar Ca(OH)2 crystal, and needle-stick ettringite were clearly
visible, hydration products overlapped with each other, and holes and
cracks were significantly reduced, resulting in the formation of dense
network structure. After hydration for 90 days (Fig.␣12 (c)), the hy­
dration products generally increased, and specific hydration products
could not be distinguished. The overall microstructure was compact,
which is consistent with the improvement of macroscopic mechanical
properties with the extension of curing age.
3.3.2. XRd
The XRD spectra of the sample prepared using different WGP particle
sizes at a curing age of 28 d are shown in Fig.␣13. The main crystal
substances were CH, SiO2 (S), calcium silicate (C2S), tricalcium silicate
(C3S), a small content of ettringite (E), as well as CaCO3 (CC) and CaSO4
(G) crystals. The peaks of CH in the XRD spectra were found at 18.00 2θ
◦
10
Construction and Building Materials 324 (2022) 126531
◦ ◦ ◦
(d = 4.9092 A), 34.10 2θ (d = 2.6270 A), and 47.12 2θ (d = 1.9268 A)
◦ ◦
[35–36]. As show in the XRD spectra, the intensity of CH at 2θ = 34.10◦
weakened as the WGP particle size increased; in particular, the peak
intensity of CH reached a minimum value when WGP III was incorpo­
rated. This may imply that when the particle size of WGP was larger,
either none of the CH or an extremely small content of it underwent a
secondary hydration reaction with the active ingredients of WGP.
Furthermore, WGP appeared in the hydration system in the form of
micro-aggregates, and the activities of WGP I and II were low.
The XRD spectra of the sample prepared with different WGP content
at a curing age of 28 d are shown in Fig.␣14. The hydration products of
the pure cement gel system and the gel system containing WGP were
similar. It was observed that the peak intensity of C2S and C3S decreased
◦
gradually at 32.60 2θ (d = 2.7445 A) as the WGP content increased. The
◦
peak intensity of CH was lower in the blended mortar than in the control
specimen. The XRD spectra show that the intensity of CH decreased as
the WGP content increased, and the lowest peak intensity of CH was
recorded when the WGP content was 20%. This is attributed to the
consumption of CH in the pozzolanic reaction with SiO2 contained in
WGP to produce a C–S–H gel; however, the C–S–H gel is an amorphous
Q. Li et al. Construction and Building Materials 324 (2022) 126531

Fig.␣12. SEM images of blended mortar with WGP III 20% content at different curing ages.

Fig.␣13. The XRD spectra of the sample with different WGP particle sizes.
Fig.␣14. The XRD spectra of the sample with different WGP content.

substance, and its peak intensity is weak in the XRD spectra and hence
consumed in the volcanic ash reaction.
cannot be characterized precisely, as reflected in the TGA–DTG curve
Fig.␣15 shows that the peak intensity of CH of the sample increased
below. A SiO2 peak was not observed in the pure cement gel, but it was
with the curing age, which is attributed to the increase in the hydration
clearly observed in the gel containing WGP. As the WGP content
degree of cement with the curing age. However, the opposite variation
increased, the peak intensity of SiO2 gradually increased at 26.64◦
◦
in CH peak intensity with curing age was observed in the gel and
(d = 3.3435 A), but the increasing amplitude was not significant. This is blended with WGP III. This may be attributed to the fully stimulated
attributable to two reasons: First, the content of SiO2 in the entire gel activity of the WGP by the alkaline hydration products as the curing age
system increased with the WGP content. Second, a portion of SiO2 was progressed, and the consumption of CH to produce a C–S–H gel of higher

11
Q. Li et al.
Fig.␣15. The XRD spectra of the sample at different curing ages.
strength. This is consistent with the conclusion that the mechanical
properties of blended mortar containing WGP III improved with the
curing age.
3.4. TGA analysis
The DTG curve can be obtained from the first derivative of the TGA
curve with respect to temperature, which represents the relationship
Fig.␣16. TGA–DTG curves of blended mortar with different WGP particle sizes (WGP content 20%, curing age 28 d).
12
Construction and Building Materials 324 (2022) 126531
between the weight loss rate and temperature. The results of TGA–DTG
analysis performed on the blended mortar with different WGP particle
sizes, WGP content, and three curing ages are shown in Figs.␣16–18,
respectively. The mass loss between RT and 100 ◦ C, as shown in the TGA
curve, was due to the departure of free water from the concrete [37]. The
mass loss that occurred between 100 ◦ C and 150 ◦ C was attributed to the
loss of combined water due to the dehydration of the C–S–H gel, which
in fact corresponded to the first strong endothermic peak in the DTG
curve. Between 150 ◦ C and 200 ◦ C, the mass loss of ettringite occurred.
Meanwhile, between 400 ◦ C and 450 ◦ C, the mass loss of CH occurred
during dehydration, and a second strong endothermic peak was
observed in the DTG curve [38]. Between 600 ◦ C and 650 ◦ C, the third
endothermic peak appeared in the DTG curve. At this time, CaCO3 began
to decompose and decarbonized into CaO and CO2 overflows.
Figs.␣16–18 show that the three factors, namely, WGP content,
particle size, and curing age, did not significantly affect the peak
emergence trend of the TGA–DTG curves of each sample; however, they
significantly affected the mass loss for the same temperature range.
The mass loss in different temperature ranges and the total mass loss
of the blended mortar, as calculated from the TGA curves, are shown in
Figs.␣19–21. The combined water constituting the mass loss from RT to
400 ◦ C was due to the departure of various hydration products, such as
C–S–H gel and ettringite. However, as shown in the DTG curve,
compared with the peak at approximately 100 ◦ C, the peak at approxi­
mately 150 ◦ C was extremely weak, and the characteristics of the peak in
the DTG curve were ambiguous; hence, it can be disregarded. Therefore,
to some extent, the mass loss in this temperature range can reflect the
content of C–S–H gel produced. The content of C–S–H gel included the
content of C–S–H gel generated by both cement hydration and the
Q. Li et al.
Fig.␣17. TGA–DTG curves of blended mortar with different WGP content (WGP III, curing age 28 d).
secondary reaction of WGP volcanic ash. As stated earlier (Sec­
tion␣2.3.3), the obtained results of TGA were used to estimate the CH
content in the blended mortar using Eq. (1), as shown in Fig.␣22.
Based on a comparison of the different particle sizes of the mortar
specimen, Fig.␣19 shows that the mass loss of the blended mortar con­
taining WGP III was the most significant in the temperature range be­
tween RT and 400 ◦ C. The departure of combined water as a result of the
dehydration of the C–S–H gel in the WGP III mortar was 37.0%, 10.7%,
and 4.1% higher than that in WGP I, II, and IV, respectively. This in­
dicates that the gel containing WGP III contained the highest content of
C–S–H gel, which was primarily due to the secondary hydration of WGP.
13
Construction and Building Materials 324 (2022) 126531
Compared with the other WGP particle sizes, the CH content of the WGP
III mortar was the lowest, i.e., lower than that of WGP I, II, and IV by
15.9%,13.7%, and 7.9%, respectively (as shown in Fig.␣22). A higher
content of consumed CH was rehydrated with WGP and formed a higher
content of C–S–H gel in the WGP III mortar, as indicated by the results of
compressive strength (highest of mortar with WGP III) and the peak
strengths of CH and SiO2 in the XRD patterns.
As shown in Fig.␣20, the mass loss of the blended mortar with 15%,
20%, and 25% WGP III content was 3.7%, 9.5%, and 1.7% higher than
that of the control specimen in the temperature range between RT and
400 ◦ C, respectively, which can be explained by the blended mortar with
Q. Li et al.
Fig.␣18. TGA–DTG curves of blended mortar at different curing ages (WGP content 20%, WGP III).
Fig.␣19. Mass loss of blended mortar with various WGP particle sizes in
different temperature ranges.
20% WGP III being the highest content in the C–S–H gel. Fig.␣22 shows
that the CH content of the blended mortar containing 15%, 20%, and
25% WGP III was 13.7%, 17.3%, and 15.02% lower than that of the
control specimen. The decrease in the content of CH was attributable to
the following two factors: In addition to being consumed by the sec­
ondary hydration via the WGP, the increase in the amount of WGP
resulted in the decrease in the amount of cement, which reduced the
amount of calcium hydroxide. Hence, the lowest CH content in the hy­
dration product imply that the WGP III content of 20% exhibits the best
14
Construction and Building Materials 324 (2022) 126531
Fig.␣20. Mass loss of blended mortar with various WGP content in different
temperature ranges.
pozzolanic activity, and this is consistent with the results of the XRD
analysis of the calcium hydroxide peak intensity for different WGP
content.
As shown in Fig.␣21, the mass loss increased by 13.6% from curing
age 7 d to 28 d in the temperature range between RT and 400 ◦ C,
whereas the mass loss increased by 42.6% from curing age 28 d to 90 d.
This is because the increase in the C–S–H gel content from 7 d to 28
d was primarily due to the hydration of cement, whereas the increase in
the C–S–H gel content from 28 d to 90 d was primarily due to the
Q. Li et al. Construction and Building Materials 324 (2022) 126531

Table␣4
Characteristics of Main Absorption Peaks of FTIR spectrum.
Vibration band Wave number (cm− 1)

Bending vibration of Si–O、Al–O [39,40] 460–474

Bending vibration of Al–O–Si [39] 681–694
Antisymmetric stretching vibration of Si–O–Si、Al–O–Si 971–1054
[40]
Stretching vibration of O–C–O [41] 1445
Bending vibration of O–H (H2O) [39] 1633–1650
Stretching vibration of O–H (CH) [42] 3450

Fig.␣21. Mass loss of blended mortar with various curing ages in different
temperature ranges.

Fig.␣24. The FTIR spectra of blended mortar with different WGP content.

Fig.␣22. The content of CH in each specimen.

Fig.␣25. The FTIR spectra of blended mortar at different curing ages.

content decreased by 3.4% from 7 d to 28 d of curing, whereas it

decreased by 9.96% from 28 d to 90 d of curing.

3.5. FTIR analysis

Fig.␣23 shows the effect of the WGP particle size on the infrared
Fig.␣23. The FTIR spectra of blended mortar with different WGP particle sizes.
vibration band of the blended mortar, and the main vibration bands are
listed in Table␣4. The stretching vibration of Si–O–Si bond in C–S–H gel
secondary hydration of the WGP. This indicates that the activity of the
at WGP I appeared at 971 cm− 1. As the decrease of WGP particle size, the
WGP in the later curing period can significantly increase the C–S–H gel
intensity of the signal at approximately 971 cm− 1 increased signifi­
content. In fact, this conclusion is supported by the CH content at all
cantly, Si–O–Si bonds migrated 981, 1047 and 989 cm− 1 when WGP II,
curing ages (as shown in Fig.␣22), as well as by the fact that the CH
WGP III and WGP IV were incorporated, respectively. This implies that a

15
Q. Li et al.
smaller WGP particle size results in a higher content of C–S–H gel in the
hydration products, and the maximum content of the C–S–H gel was
indicated for blended mortar containing WGP III. The O–C–O bond of
CO32– had a stretching vibration absorption peak at approximately
1445 cm− 1. CO32– was generated by the carbonization of a sample
exposed to air. Therefore, the O–C–O bond absorption peak was
observed in both the pure cement slurry and WGP-doped composite gel
slurry.
Fig.␣24 shows the effect of the WGP content on the infrared vibration
band of the blended mortar. The peak intensities of the Si–O and Al–O
bonds increased in the vibrational band between 460 and 474 cm− 1 as
the WGP content increased. By contrast, the Si–O–Si bond vibration
signal appearing at 983 cm− 1 shifted to higher wavenumbers as the WGP
content increased; when the WGP content was 10%, 15%, and 20%, the
band shifted to 995, 993, and 1047 cm− 1, respectively. However, the
WGP content was 25%, the band moved to 989 cm− 1. It was reported
previously that the migration to high wavenumbers indicates the
gradual polymerization of Si–O bonds into Si–O–Si bonds, which can
increase the polymerization degree of the Si–O tetrahedron in the C–S–H
gel [43]. The O–H bond of the vibration signal of hydration product CH
appeared at 3450 cm− 1, and the peak area decreased as the WGP content
increased, indicating that the content of hydration product CH was the
highest in the pure cement gel.
Fig.␣25 shows the effect of the different curing ages on the infrared
vibration band of the blended mortar. The intensity of the signal at
approximately 973 cm− 1 was the lowest at 7 d of hydration. The
wavenumber of the band shifted to a higher frequency as the reaction
advanced, and the band shifted to 1024 and 1047 cm− 1 at 28 d and 90
d of curing, respectively. Moreover, the signal at approximately
973 cm− 1 was wider in the 28 d and 90 d specimens than that in the
initial 7 d specimen. The increase in the peak area indicates that the
WGP activity was more significant in the later curing period.
4. Conclusion
Through compressive strength test, the influence of WGP particle
size, WGP content and curing age on the mechanical properties of
blended mortar was analyzed. The mechanism of the above three factors
on the activity of WGP pozzolanic was discussed by microscopic
experiment, FTIR and TGA–DTG, the following conclusions have been
drawn from the present study:
a) The fluidity of the mortar containing WGP I and II was higher than
that of the control group, but the bleeding was severe. The mortar
incorporated with WGP III indicated higher segregation resistance
than the other groups, and the segregation resistance of the mortar
containing 20% WGP III was 4.8% higher than that of the control
group. The fluidity of the mortar containing WGP IV was lower than
that of the control group, which was attributed to the larger specific
surface area.
b) The compressive strength of the blended mortar first increased and
then decreased as the WGP particle size decreased. The compressive
strength of the mortar containing WGP I and II at all curing ages was
lower than that of the control specimen. The compressive strength of
the mortar containing WGP III was lower than that of the control
group on curing 7 d, but it increased as the WGP III content increased
at later curing days. The compressive strength of the mortar con­
taining 20% WGP III was 3.5% and 9.6% higher than that of the
control sample at 28 d and 90 d, respectively. Equations (3)–(5) can
be used to better predict the relationship between the WGP particle
size and WGP content against the compressive strength.
c) For the same WGP content, SEM revealed that the internal structure
of the WGP III mixed mortar was the densest. The peak intensity of
CH was the lowest in the blended mortar containing WGP III, and the
CH content in the WGP III mortar was lower than that in the WGP I,
WGP II, and WGP IV mortars by 15.9%, 13.7%, and 7.9%,
16
Construction and Building Materials 324 (2022) 126531
respectively, based on the TGA results. Furthermore, the reduction in
combined water as a result of the dehydration of the C–S–H gel was
the highest in the blended mortar containing WGP III. Based on the
SEM and EDS experimental analysis, WGP III demonstrated better
activity than the other WGP particle sizes, which is consistent with
the conclusions of macroscopic mechanics.
d) For the blended mortars containing 0%–25% WGP III, the SEM re­
sults revealed that the microstructure of the cement slurry containing
20% WGP III was the densest. In the mixed mortar containing 20%
WGP III, the peak intensity of CH in the XRD spectrum and the mass
loss calculated by TGA as a result of dehydration of the mortar
indicated the lowest CH content. The mass loss (RT temperature to
400 ◦ C) of the mortar mixed with 20% WGP was 9.5% higher than
that of the control specimen, which indicates that the content of the
C–S–H gel was higher when the mortar contained 20% WGP III.
Considering the fluidity test, mechanical strength test, and micro-
mechanism analysis, a WGP III content of 20% is recommended as
the best content.
e) The FTIR results revealed that when the WGP content was 20% and
the WGP particle size was III, the signal intensity of the Si–O–Si bond
was the most significant, and the O–H bond peak area of the vibra­
tion signal of the hydration product CH was the smallest, indicating
that the secondary hydration rate of blended mortar was the fastest,
and the content of hydration products such as C–S–H gel was the
highest. In addition, the pozzolanic activity of the WGP increased as
the curing age increased.
CRediT authorship contribution statement
Qiong Li: Writing – original draft, Writing – review & editing,
Methodology, Investigation. Hongxia Qiao: Conceptualization, Vali­
dation, Formal analysis. Aoyang Li: Conceptualization, Validation,
Formal analysis. Guanjun Li: Supervision, Data curation.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgements
The authors would like to express their gratitude to the National
Natural Science Foundation of China (Nos. 52178216, 51868044).
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