Construction and Building Materials 299 (2021) 123900

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Construction and Building Materials

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Properties of cement mortar containing recycled glass and rice husk ash
Salifu Nasiru a, Linhua Jiang a,⇑, Lin Yu a, Hongqiang Chu a, Yu Huang b,⇑, Chun Pei c, Yue Gu a,
Weizhun Jin a, Edwin Eyram Klu a, Ming-Zhi Guo a,⇑
a
College of Mechanics and Materials, Hohai University, Nanjing 210098, China
b
Institute of Earth Environment, Chinese Academy of Sciences, Xi’an, China
c
Key Laboratory of Durability for Marine Civil Engineering, College of Civil and Transportation Engineering, Shenzhen University, Shenzhen 518060, China

h i g h l i g h t s g r a p h i c a l a b s t r a c t

Combined use of waste glass and RHA

greatly alleviates wastes disposal at
landfills.

Use of RHA improved mechanical and
durability of cement mortar.

Addition of RHA suppressed RG-
induced ASR expansion.

RHA holds great promise as eco-
friendly pozzolanic materials.

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

Article history: Using recycled glass (RG) to replace river sand in the production of cement-based materials saves the
Received 28 January 2021 increasingly depleting natural sand resources. Previous studies have shown that the smooth surface
Received in revised form 29 April 2021 and reactive silica of RG adversely affected its bonding with the cement paste and thereby caused a
Accepted 6 June 2021
potential alkali-silica-reaction (ASR). This study used rice husk ash (RHA) as an eco-friendly mineral
Available online 17 June 2021
admixture to ameliorate the properties of the RG incorporated mortar. A fixed replacement of 50% RG
was used to replace sand, while varying proportions (10%, 20% and 30%) of RHA were adopted to replace
Keywords:
cement. For comparison, a mixture containing only sand and cement was used as the reference sample.
Recycled glass
Rice husk ash
The flexural and compressive strength, water absorption, ASR expansion, and rapid chloride mitigation
Pozzolanic reaction (RCM) of the hardened samples were evaluated. In addition, SEM, XRD, and TG analysis were employed
ASR to analyze the microstructures and chemical compositions of different samples. The results showed that
Cement mortar incorporating RG as a river sand replacement in cement mortar reduced flexural and compressive
strength and increased water absorption and chloride ion penetration. Moreover, the ASR expansion
value (0.34%) was beyond the permissible limit (0.1) indicated by the ASTM C1260. The addition of
RHA improved the mechanical properties and durability of the cement mortar at a later curing age as
a result of the RHA-induced pozzolanic reaction and micro-filler effect. By converting portlandite (CH)
derived from cement hydration into secondary C-S-H, the use of RHA greatly reduced the porosity (aug-
menting the compressive and flexural strength) and concurrently suppressed the RG-induced ASR expan-
sion. The results of XRD, SEM and TG analysis corresponded well with the macro-property analysis and
helped to elucidate the underlying mechanisms of the RHA-induced beneficial effects. Findings from this
study provide new insights into the potential use of eco-friendly RHA in addressing the mechanical and
durability problems associated with the use of RG as aggregate in cementitious materials.
Ó 2021 Elsevier Ltd. All rights reserved.

⇑ Corresponding authors.
E-mail addresses: hhulhjiang@163.com (L. Jiang), huangyu@ieecas.cn (Y. Huang), mz.guo.mz@connect.polyu.hk (M.-Z. Guo).

https://doi.org/10.1016/j.conbuildmat.2021.123900
0950-0618/Ó 2021 Elsevier Ltd. All rights reserved.
S. Nasiru, L. Jiang, L. Yu et al.
1. Introduction
Waste glass accounts for approximately 7% of the 200 million
tons of solid wastes generated worldwide as estimated by the Uni-
ted Nations [1]. Different from other waste products, waste glass is
non-degradable and thus exerts a great burden on the environ-
ment. Hence, effectively recycling of waste glass becomes increas-
ingly necessary and vital to maintain the overall sustainability of
the environment, especially for countries and regions without glass
manufacturing industries. Attempts have been made to recycle
waste glass as various products, such as abrasives, sand-blasting,
aggregates, reflective paints in the form of beads for highways,
fiberglass, and fractionators [2].
Similar to natural river sand, most of recycled glasses (RG) con-
sist of more than 70% SiO2. Thus, RG is generally used in concrete or
mortar as a replacement of fine aggregate. Extensive studies have
employed RG as alternative aggregates to produce various con-
struction materials [3–5]. Moreover, RG with a particle size of less
than 140 lm can be used to replace cement due to its pozzolanic
potential in a finer powder form [6]. The RG-induced pozzolanic
effect is conducive to suppressing alkali-silica reaction (ASR) [7–
10]. However, using RG to replace natural sand is not without lim-
itations. The primary drawback is that the weak bonding between
the RG’s smooth surface and the cement matrix gives rise to a
higher porosity and a lower strength [11–14]. Another major draw-
back is the potential ASR between the silica-rich glass and the
alkali in the cement [15–17]. Swelling of the produced ASR gel
upon absorbing water causes severe damages on the concrete cov-
ers and structures, leading to the ingress of foreign aggressive ions
and subsequent freeze–thaw and corrosion-related deterioration
on the durability [18]. This is especially true when the RG replace-
ment exceeds 50%, the ASR becomes more significant with a much
higher expansion (0.7%). Therefore, special caution is needed if the
RG replacement rate is above this threshold [19–21]. These
observed drawbacks, to a wider extent, greatly limit the use of
RG as fine aggregates in the construction industry. Fortunately,
the addition of appropriate mineral additives with pozzolanic
activities in the RG incorporated products is conducive to address-
ing the ASR caused problems [22–24]. In addition, the incorpora-
tion of RG in concrete leads to a decrease in unit weight, mainly
due to a lower density of glass as compared to natural sand. It
was reported that water absorption decreased with increasing
the content of RG as a result of the non-hygroscopic nature of glass
[25].
Recently, cementing materials, especially by-products from the
industry and agricultural processes (as diverse as fly ash, ground
granulated blast furnace slag, silica fume and rice husk ash, sugar
cane bagasse ash, bamboo leave ash), have been used to improve
the properties of concrete and mortar. Unlike industrial by-
product pozzolanic materials, natural pozzolanic materials are
mostly obtained by calcination at appropriate temperatures. Poz-
zolans exert both filler and pozzolanic effects on the properties
of concrete [26]. The effectiveness of pozzolans is highly dependent
on their chemical and physical characteristics.
Rice husk is a by-product derived from the rice milling industry.
The husk mainly consists of lignin, cellulose and silica [27]. Rice
husk ash (RHA) is obtained from the combustion of rice husk. Upon
combustion, about 20% (by weight) of the burnt husk is retrieved in
the form of ash. The formation of RHA with over 80% amorphous
silica can be obtained at a combustion temperature below 700 °C
[28,29]. Apart from burning temperatures, the combustion rate
and duration, as well as the cooling process, will also have an
impact on the quality of RHA. For example, slow cooling with an
average oxygen supply favors the formation of amorphous silica,
while a high supply of oxygen (oxidizing environment) results in
2
Construction and Building Materials 299 (2021) 123900
the formation of crystalline silica. RHA with amorphous silica has
a more porous structure with a large surface area and thereby is
more reactive. In addition, the reactivity of RHA increases with
an increase in the fineness [30].
The use of RHA as a pozzolanic material in replacement of
cement has been well investigated and holds several advantages
[31]. This replacement rate of RHA is influenced by factors such
as the fineness of the ash, nature of the produced silica and the
presence of other materials like carbon [7]. A partial replacement
of cement by reactive RHA reduces the cement production emitted
CO2 [32]. In addition, the incorporation of 10%30% RHA in con-
crete improves the compressive strength at a later curing age
[33]. Furthermore, RHA is also employed to suppress the ASR-
incurred expansion in concrete samples. This is because in the
presence of water, the reactive silica from RHA reacts with port-
landite (CH) to produce more secondary C-S-H gel as shown in
Eq (1) [33]. This leads to less availability of soluble calcium to react
with the dissolved silica, thereby decreasing the alkalinity in the
concrete. The generation of additional C-S-H gel contributes to
the improvement in the strength and durability of the RHA incor-
porated concrete/mortar. Porosity, corrosion resistance and freeze
thaw of concrete and mortar are improved with the addition of
RHA, mainly due to the filler effect. Additionally, the addition of
RHA in concrete or mortar leads to a reduction in density due to
its low density nature [34].
SiO2 þ CaðOHÞ2 þ H2 OÒCaO  SiO2  H2 O ð1Þ
Silica CH (C-S-H)
To date, however, few studies have focused on the use of RHA to
improve the mechanical properties and durability of cement mor-
tar using RG as sand replacement. This study employed RHA as a
replacement of cement at varying ratios of 10%, 20% and 30% to
produce cement mortars prepared with RG in replacement of 50%
river sand. The influence of RHA on the properties of cement mor-
tars was analyzed. Additionally, SEM, XRD and TG analysis was
performed in an attempt to dissect the primary mechanisms
underlying the observed influence on the mechanical property
and durability.
2. Experimental
2.1. Materials
Natural sand and RG were employed as fine aggregates. Natural
sand was purchased from a local dealer with varying sizes. RG
(mostly beer bottles) was collected from a local restaurant. The col-
lected RG was crushed using a mechanical crusher and then sieved
to the desired sizes. The crushed glass particles were washed to get
rid of all impurities, followed by oven-dry at 105 °C for 24 h to
evaporate the water completely. The particle size distribution
(PSD) of RG and sand is shown in Fig. 1. The fineness modulus
(FM) of RG and sand was 2.8 and 2.3, respectively.
The rice husk was first obtained from a local rice milling com-
pany in Nanjing, China. The husk was burnt in an open furnace
for 1 h. The uncontrolled burning generated RHA with a black
appearance and a higher LOI value of 13.3%, which exceeded the
ASTM requirement, indicating the presence of an excessive amount
of carbon, which was undesirable for an effective pozzolan. The
RHA was then submitted to a recalcination procedure to reduce
the LOI value as well as the carbon content. The black colored
ash was placed in a special furnace in the laboratory and subjected
to heating at a rate of 200 °C per hour until it reached a desired
temperature of 650 °C over a period of 3 h and 15 min. At
650 °C, the temperature was kept constant for a burning time of
S. Nasiru, L. Jiang, L. Yu et al. Construction and Building Materials 299 (2021) 123900

Table 2
Chemical and physical properties of cement and RHA.

Chemical composition (wt%) Cement RHA

SiO2 20.50 91.90
Al2O3 5.61 0.278
Fe2O3 3.84 0.188
CaO 62.83 1.15
MgO 1.70 0.711
K2O 1.31 3.99
Na2O 0.135 0.0350
TiO2 0.294 0.0260
SO3 3.07 0.215
Loss on ignition – 6.7
Physical properties
45 lm fineness passing 99.80 99.08
Average particle size (lm) 13 18
Color – Dark gray

Fig. 1. PSD curve of RG and sand.

1 h. This procedure was similar to the one used in a previous study

[35]. The ash was then pulverized to fine powder using a ball mill.
X-ray fluorescence analysis (XRF) was used to analyze the
chemical compositions of RG, RHA and cement. The results
obtained for RG is presented in Table 1. Table 2 provides the chem-
ical composition and physical properties of RHA and cement.
The PSD of cement and RHA was analyzed by a laser particle
size analyzer (GSL-IOIBI) in a liquid state. RHA and cement were,
respectively, dispersed in water and ethanol using a KQ218 ultra-
sonic treatment machine. The obtained PSD of RHA and cement
is presented in Fig. 2.

2.2. Mix proportions

The mortar samples were prepared with a water to binder (w/b) Fig. 2. PSD curve of RHA and cement.
ratio of 0.5 and a binder to aggregate (b/a) ratio of 1:3. The sand
was replaced by RG at a percentage of 50% (by weight). RHA was
added to replace cement at varying ratios of 10%, 20% and 30%. the samples were demolded, labeled, immersed in water, and
For comparison, the control sample with 100% sand and without stored in a curing room until the age of testing.
the addition of RHA (OPC) was also prepared. Table 3 gives the
detailed mix proportions for all the samples. 2.4. Characterization

2.3. Sample preparation The crystalline phase mineralogy of the well pulverized RHA
was analyzed by an automated general-purpose X-ray diffraction
First, dry materials were mixed for 2 min in an automatic instrument (XRD, Ultima IV). The 2h scanning range was from 10
mechanical mixer (JJ-5 cement mortar mixer conforming with to 80° with a scanning speed of 5°/min. The obtained results were
ISO 679), followed by the addition of the appropriate amount of then analyzed using Jade 5.0.
water and further mixed for another 2 min. Then, the fresh mix- The XRD patterns of RHA are shown in Fig. 3. The higher sharp
tures were casted into steel molds, followed by compacting on a peak at around 22° was the characteristic peak of a-cristobalite
mechanical vibrating table for 1 min. The surface of the molds (high-temperature phase of SiO2). Generally, the crystalline phases
was covered with plastic sheets to prevent water loss. After 24 h, appear as sharp peaks in the diffractogram, while the amorphous
phases existed as a single broad peak. Considering that the area
under the broad peak was significantly greater than the under the
Table 1
crystalline peaks, the re-calcinated RHA consisted primarily amor-
Chemical properties of RG.
phous SiO2. This was in good agreement with a previous study [36].
Chemical compositions (wt%) RG The morphology of RHA and mortar samples was characterized
SiO2 68.43 using a scanning electron microscopy (SEM, JEOL Model JSM-
Al2O3 2.59 6490). Fig. 4 shows the SEM image of the re-calcinated RHA. It
Fe2O3 0.375 can be seen that predominantly small particles were obtained
CaO 11.28
MgO 1.22
under a controlled burning and grinding condition, indicating a
K2O 0.598 high specific surface area. A few large particles with irregular
Na2O 14.77 shapes were also obtained. The predominant proportions of small
TiO2 0.0647 RHA particles guaranteed a good pozzolanic property as reported
SO3 0.187
by [37].
3
S. Nasiru, L. Jiang, L. Yu et al. Construction and Building Materials 299 (2021) 123900

Table 3
Mix proportions (in grammes) of mortar samples.

Mix Mix Notation Cementitious materials Fine aggregates Water

(binder)
Cement RHA Sand RG
Control C 450 – 1350 – 225
50%RG M1 450 – 675 675 225
RHA10% – 50%RG M2 405 45 675 675 225
RHA20% – 50%RG M3 360 90 675 675 225
RHA30% – 50%RG M4 315 135 675 675 225

In order to determine the closeness of the strength values of the

RG incorporated mixes to that of the control, strength activity
index (SAI) was determined in accordance with ASTM C311 [40],
which can be calculated by (Eq. (2)):
A
SAI ¼ x100: ð2Þ
B
Where, A and B are the average compressive strength of the
RHA incorporated sample and the control sample, respectively.

2.5.3. Water absorption

Fig. 3. XRD patterns of RHA.
The water absorption test was carried out at 28 d in accordance
with ASTM C642 [41]. The sample was oven-dried at 105 °C for
24 h to reach a constant weight. The initial weight of the oven-
dried sample was determined. After that, the dried sample was
allowed to cool down at room temperature for another 24 h, fol-
lowed by placing in cold water for a period of 24 h. During this pro-
cess, the sample was taken out from the water bath and re-
weighted after 30 min and 24 h. Initial surface absorption (ISA)
and final water absorption (FSA) were calculated by Eq. (3) and
Eq. (4):
ðW30min  WodÞ
ISA ¼ x100 ð3Þ
Wod

ðW24h  WodÞ
FWA ¼ x100 ð4Þ
Wod
Where, W30min is the weight of the sample after 30 min of
immersion, (g); W24h is the weight of the sample after 24 h of
immersion, (g); Wod is the weight of the oven dried sample.

2.5.4. Rapid chloride mitigation (RCM)

Fig. 4. SEM image of RHA.
2.5. Testing methods
2.5.1. Flexural strength
Flexural strength test was conducted at 7 and 28 d in compli-
ance with ASTM C348 [38]. The prism specimens
(40  40  160 mm) were tested in a universal testing machine
(50 KN) with a constant loading speed of 50 N/s.
This experiment was done following the procedures stipulated
in GB/T 50082-2009 using a NJ- RCM concrete chloride diffusion
coefficient tester, modeled after Nordest test method NT build
492. The sample was 50 mm thick slices cut from a
U100  200 mm cylinder. The lateral surface of the obtained sam-
ples was sealed with an epoxy resin to ensure the one-dimensional
flow of chlorides in the disc. The experimental setup consisted of
an anolyte (0.3 M NaOH solution) and a catholyte (10% NaCl solu-
tion). The RCM test was run for a duration determined by the spec-
imen’s initial current with an applied voltage of 30 V. After the
RCM test, the specimen was split into two halves, followed by
spraying 0.1 N of AgNO3 solution on the fractured surface. The
reactions leading to the formation of the color zones are as follows:
Ò
Agþ þ Cl AgCl ðSilvery whiteÞ ð5Þ

Agþ þ OH ÒAgOHÒAg2 O ðBrownÞ ð6Þ

2.5.2. Compressive strength/strength activity index
Compressive strength test was conducted in compliance with
ASTM C349 [39]. The compressive strength was measured by a
hydraulic compression testing machine with a maximum loading
capacity of 600 kN on the remaining halves of the prisms broken
in the flexural strength test at 7 and 28 d.
4
The depth of the chloride penetration was measured as the
average of seven measurements across the width of the specimen,
neglecting the 10 mm end of each side. Diffusion coefficient was
then calculated based on the chloride penetration, sample thick-
ness, exposure time, voltage and average sample temperature.
S. Nasiru, L. Jiang, L. Yu et al. Construction and Building Materials 299 (2021) 123900

2.5.5. Alkali-silica reaction (ASR)

The ASR caused expansions in mortar bar samples
(25  25  285 mm) were determined according to ASTM C1260
[42]. In this method, by immersing during 14 d the mortar bar
samples in a hot (80 °C) sodium hydroxide (NaOH) water solution,
the ASR reaction is enhanced. As initial measurement (zero read-
ing), expansions of the samples are taken after immersing them
in a hot (80 °C) water bath during 24 h. Length changes of the bars
were then taken at 1, 4, 7, 10, 12 and 14 d using a length compara-
tor by taking the samples out (max. 15 s) of the NaOH water solu-
tion. Finally, the difference between the zero reading of one
specimen and the reading at each period is the expansion of the
specimen for that period. An expansion of 0 to 0.1% gives an indi-
cation of not being harmful or reactive. A 0.1 to 0.2% expansion is
considered to be either harmful or deleterious and would need fur-
ther testing. An expansion of above 0.2% is regarded as being reac-
tive or deleterious.

2.5.6. XRD analysis

An Ultima IV diffractometer with a Cu Ka radiation was used to
determine the mineralogy of the hardened samples after 28 days of
curing. Prior to XRD analysis, the samples were crushed and
ground into powders using a mortar and pestle. The 2h scanning
range was from 5° to 90° at a speed of 5°/min.
Fig. 5. Flexural strength of mixes at different curing ages.
pozzolanic reaction (especially, at a higher dosage), as well as the
packing ability [45]. Similar results were reported previously [46].

2.5.7. SEM observation 3.2. Compressive strength

The microstructures of the samples after 28 days of curing were
examined using scanning electron microscopy (SEM, Zeiss Sigma
300), with 0.02 – 30kv accelerating voltage.
2.5.8. Thermal gravimetric and differential thermal gravimetric
analysis (TG-DTG)
The consumption of CH due to the RHA-induced pozzolanic
reaction after 28 days of curing was evaluated by thermal gravi-
metric (TG) and differential thermal gravimetric (DTG) analysis
using a Netzch STA 449C, Jupiter equipment. The finely ground
paste samples were heated over a range of 33°C to 1000 °C at a rate
of 20°C/min in a nitrogen atmosphere.
3. Results and discussion
3.1. Flexural strength
The 7 and 28 d compressive strength of different samples is pro-
vided in Fig. 6. Similar to the trend of flexural strength, the com-
pressive strength of all the RG incorporated samples was
decreased compared with the control sample (C, 24.09 MPa) at 7
d. Increasing the RHA content resulted in a corresponding decrease
in the compressive strength. The diluting effect caused by the
replacement of cement by RHA mainly contributed to the compres-
sive strength reduction. This finding was consistent with a previ-
ous study which also reported that the addition of RHA to
replace 10%-30% cement led to an increase in the volume of capil-
lary pores at the early phase, resulting in a more porous structure
as compared to the reference sample [47].
At 28 d, the compressive strength of M1 still suffered a 5%
decrease compared with C (25.04 MPa). The addition of RHA in
the RG incorporated samples improved the compressive strength.
M3 and M4 even experienced a 4.4% and 7.5% increase in the com-

The 7 and 28 d flexural strength of different samples is shown in

Fig. 5. The 7 d flexural strength of the control sample was 5.30 MPa.
Compared with the control sample (C), the flexural strength of M1
(with 50% RG and without RHA) decreased by 13.2%. This was
ascribed to the weak bonding between the smooth glass interface
and the cement paste. The addition of RHA in the RG incorporated
mortars (M2, M3 and M4) failed to improve the flexural strength at
an early curing age. Similar results were reported in previous stud-
ies which also observed a decrease in flexural strength with
increasing the replacement percentage of RHA at early ages
[43,44]. This was because the addition of RHA to partially replace
cement reduced the amount of alite (C3S), which is a main contrib-
utor to the early strength development.
At 28 d, the flexural strength of M1 still experienced a 15.2%
reduction compared with C (6.32 MPa). Compared with M1, the
use of RHA improved the flexural strength in a dosage-dependent
manner. For example, the flexural strength of M2, M3 and M4
increased by 10%, 27.2% and 30.8%, respectively. It was worth not-
ing that M3 and M4 even gained a 7.9% and 10.9% increase in the
flexural strength, respectively, compared with C. Such an improve-
ment in flexural strength was probably due to the RHA induced Fig. 6. Compressive strength of mixes at different curing ages.

5
S. Nasiru, L. Jiang, L. Yu et al.
pressive strength, respectively, compared with C. Compared with
M1, M3 and M4 gained a 9.9% and 13.2% increase in compressive
strength, respectively. It is noteworthy that the 28-d compressive
strength of C, M3 and M4 even exceeds the 25 MPa limit stipulated
by European Standard EN 1504, meaning that they can be consid-
ered for structural applications [48]. This strength improvement
was also attributed to the RHA-induced pozzolanic reaction, during
which process the reactive silica in RHA reacted with CH to gener-
ate secondary C-S-H gel. Consequently, the number of pores in the
mortar matrix was reduced (which will be discussed in later) [15].
Another reason may be that RHA consisting of mainly finer parti-
cles (reflected by a high specific surface area) served as nucleation
sites for cement hydration. These findings agreed well with other
published literature. For example, concrete mixes containing sug-
arcane bagasse ash (SCBA) [49] and cement mortar containing both
fly ash (FA) and RHA [29] all suffered a decrease in compressive
strength as compared to their respective control samples at 7 days.
At a later age (after 28 days), an increase in compressive strength
of the mixes incorporated with SCBA, FA and RHA was observed
as a result of pozzolanic reactions.
Fig. 7 shows the calculated SAI of the RG incorporated samples
at different curing ages. At 7 days, the strength of M3 and M4 did
not satisfy the criteria for the minimum strength activity index of
75%. Similarly, a previous study reported that the activity index of
concrete containing waste glass powder and RHA at early ages also
failed to meet the minimum strength requirement [18]. It can be
seen that SAI of the four RG incorporated mixes increased signifi-
cantly at 28 d relative to 7 d, mainly due to the delayed onset of
the pozzolanic reaction between RHA and CH. Moreover, all the
RHA incorporated samples gained more than 75% (reference line)
SAI at 28 d (97.8% and 104.4% for M2 and M3, respectively), while
M4 achieved the highest SAI of 107.5%. These findings were consis-
tent with those reported by a previous study [50]. As recom-
mended by ASTM C618, an active pozzolana should have a
minimum SAI of 75%. Thus, it can be expected that over 70% of
the added RHA can be effective in augmenting the compressive
strength of the RG incorporated samples.
3.3. Water absorption
Fig. 8 shows the ISA and FWA of different samples at 28 d of cur-
ing. The control mix (C) contained more air voids, resulting in a
high FWA (8%) but a median ISA. Compared with C, M1 had a
higher ISA but a lower FWA. The decrease in FWA was due to the
nearly zero water absorption of RG in M1 i.e. a relatively thinner
water layer was absorbed on the RG surface in a wet state [51].
Fig. 7. SAI of the RG incorporated mixes at different curing ages.
6
Construction and Building Materials 299 (2021) 123900
This observation agreed well with previous studies [52,53]. Not
much difference was observed with addition of 10%RHA (M2).
The addition of 20% RHA in the RG incorporated sample (M3)
resulted in a reduction in both ISA and FWA (2.4% and 6.6%, respec-
tively), which possessed the lowest ISA and FWA. The reduction in
porosity (as a result of pore refinement) and the corresponding
increase in density were possibly responsible for this observation.
However, further increasing the RHA content to 30% (M4), an
increase in both ISA and FWA was observed. This was probably
due to the hygroscopic nature of RHA, which increased the water
demand. It should be noted that the ISA and FWA of M4 were still
similar or lower to that of C. The results of water absorption were
in good agreement with that of the 28-d compressive strength.
3.4. Hardened density
Fig. 9 shows the hardened density of different samples at 28 d
prior to the compression strength test. Compared with C, M1,
M2, M3 and M4 had a slight decrease of 3.3%, 5.5%, 3.0% and
2.7% in density, respectively. Compare with sand (2.62 g/cm3), RG
has a lower specific gravity (2.49 g/cm3), resulting in a reduction
in mass per unit volume. This finding was insistent with a previous
study [1]. The observed decrease in hardened density of M2 (10%
RHA) was due to less dense particles of RHA compared with
cement. Interestingly, the addition of a higher amount of RHA in
the RG incorporated samples (M3 and M4) led to a slight increase
in hardened density as compared to M1. This could be due to the
micro filler effect of the added RHA and the formation of additional
C-S-H. Such an improvement in hardened density was reflected by
a corresponding increase in compressive strength as shown in Sec-
tion 3.2. The difference in hardened density between the control
sample and the RHA incorporated mixes was 3.3%, 5.5%, 3% and
2.7% for M1, M2, M3 and M4, respectively. It was also reported that
the replacement of cement by RHA decreased the density of con-
crete initially due to the less dense nature of RHA, but further
increasing the amount of RHA led to an increase in hardened den-
sity [54].
3.5. RCM
The results of chloride penetration and mitigation coefficient of
different samples after 28 d of curing is summarized in Table 4. The
Fig. 8. ISA and FWA of samples after 28 d of curing.
S. Nasiru, L. Jiang, L. Yu et al. Construction and Building Materials 299 (2021) 123900

be more effective in improving the corrosion resistance of mortar

as compared to fly ash and palm oil ash using rapid coulomb
passed test (RCPT) [56].

3.6. ASR

The ASR test results of all the mixes are shown in Fig. 11. Com-
pared with C (0.04%), M1 had an expansion of 0.34%, which was far
above the permissible limit (0.1%) indicated by the ASTM C1260, indi-
cating the significant ASR expansion caused by partially (50%) replac-
ing sand by RG. This was consistent with a previous study [53]. The
addition of RHA as an ASR suppressor in the RG incorporated samples
effectively reduced the ASR expansions. The expansions measured
(0.01–0.07%) of M2, M3, and M4 were all below the permissible limit.
The low expansion induced by the addition of RHA was possibly due
to the neutralization of excessive alkalinity by silicic acid as a result of
a controlled pozzolanic reaction [57]. Compared with M1 of this cur-
rent study, the expansion rate of M2, M3, and M4 samples decreased
by 95.95%, 80.23% and 93.89%, respectively. [58] used 40% ground-
Fig. 9. Hardened density of mixes at 28 d. granulated blast furnace slag (GGBFS) as a replacement of cement
in controlling ASR, and observed a 68% reduction in ASR expansion.
Another study employed ground clay brick (GCB) to mitigate ASR
average penetration depth range was used to calculate the mitiga- expansion and found that 25% of GCB showed good pozzolanic reac-
tion coefficient (D) using Eq. (7): tivity and helped to reduce the ASR expansion [59]. Glass powder was
rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi! also used to control the ASR expansion of mortars containing recycled
0:0239ð273 þ TÞðLÞ ð273 þ TÞLx glass aggregate (20% and 30%). It was found that the 17-mm glass
D¼ x  0:0238 ð7Þ
ðV  2Þt V2 powder had an expansion of only 0.05% (less than 0.1%) even at an
extended period of 28 days, indicating that glass powder has a good
Where, D is the non-steady-state mitigation coefficient (10-12
2 ASR mitigation ability [60].
m /s); V is the applied voltage (V); T is the average value of initial
The addition of RHA led to a higher water demand due to its
and final temperature in the anolyte solution (°C); L is the thickness
hygroscopic nature, which in turn increased the shrinkage and
of the specimen (mm); x is the average value of the penetration
decreased the expansion. For example, M2 experienced a shrinkage
depth (mm); and t is the time (h).
at an early age. The lowest expansion rate of M2 (10% RHA) was
For C, the chloride penetration depth was about 7.6 mm with a
probably attributed to the combined effects of RHA induced dilu-
mitigation coefficient of 1.6186  10-12 m2/s. M1 showed an
tion effect and pozzolanic reaction, which was also evidenced by
increase in the chloride penetration depth. An increase in the pen-
a previous study [60]. The results showed that the addition of
etration depth of M1 was accompanied by a corresponding 37.25%
10–30% RHA can be very effective in controlling the ASR expansion
increase in the mitigation coefficient compared with C. The incor-
of the RG incorporated mortar or concrete.
poration of RHA in the samples containing RG (M2, M3, and M4)
reduced the chloride penetration depth in a dosage-dependent
3.7. XRD
manner. The penetrating rate of chloride ion into mortar and con-
crete is basically dependent on the internal pore structures. Thus,
The XRD patterns of C, M1, and M4 after 28d of curing are pre-
the observed reduction in penetration depth and mitigation coeffi-
sented in Fig. 12. Typical CH peaks at 180, 340 and 50.70 were
cient of the RHA containing mixes is due to the refinement of the
observed in C and M1 along with the emergence of quartz peak
microstructures and reduction in porosity caused by the RHA-
at 26.80 (due to the presence of SiO2 in sand and RG) and calcite
induced pozzolanic reaction and micro-filler effect. Compared with
peak 29.40 (attributed to the reaction between CaO and CO2 from
C, M2, M3, and M4 experienced a 10.3%, 66.4% and 93.8% improve-
the atmosphere). Quartz and calcite peaks were also detected in
ment in the value of D, respectively. These results were in good
M4. However, no CH peak but an a-cristobalite peak at 220 (high
agreement with previous studies which reported the improvement
temperature phase of SiO2) was detected in M4, indicating the
in the impermeability of concrete to chloride attack as a result of
presence of RHA and the consumption of CH by the RHA-induced
the addition of high-dosage pozzolanic materials [35,55]. In
pozzolanic reaction. Moreover, typical alite (C3S) peaks were dis-
Fig. 10, the silvery white zone corresponded to the chloride pene-
played at 19.80 and 31.160 in C and at 32.90 and 41.310 in M1
tration depth, whiles the brown zone represented the chloride free
and M4, respectively. Meanwhile, characteristic belite (C2S) peaks
zone (with red lines separating the two distinct zones). Visual
were present at 39.60 in C, at 31.10 and 41.70 in M1, and at 36.90
inspection of these pictures further confirmed the above conclu-
and 53.10 in M4, respectively. The presence of alite and belite in
sions. Similarly, a previous study reported that RHA was found to
all the three samples revealed that the hydration process was still
not complete. It is noteworthy that the peak intensity of alite and
Table 4 belite in M4 was lower than that in M1 and C, suggesting a higher
Summary of RCM test results. hydration degree in M4. The results of the XRD analysis further
Mix Test Penetration Mitigation
supported the explanations of the improvement in the mechanical
Notation Duration(h) Depth(mm) Coefficient(10-12 m2/s) and durability properties discussed previously.
C 48 7.6 1.62
M1 48 10.1 2.22 3.8. SEM
M2 48 6.9 1.45
M3 48 3 0.54 The SEM images of C, M1, and M4 after 28d of curing are pre-
M4 48 0.9 0.10
sented in Fig. 13. Compared with C and M4, M1 had more larger
7
S. Nasiru, L. Jiang, L. Yu et al.
Fig. 10. Split surfaces of samples after spraying 0.1 N AgNO3: (a) C, (b) M1, (c) M2, and (d) M4.
Fig. 11. ASR expansion of mortar bars.
pores due to the weak bonding between the cement matrix and the
smooth surface of RG. A larger amount of needle-like ettringites
(due to the reaction between lime and alumina/sulfates) were
observed in C and M1. In contrast, almost no ettringite was
observed in M4 with the presence of more flocs-like C-S-H gel.
Moreover, in good agreement with the XRD results, CH was not
present in M4 as a result of the reaction demonstrated by Eq (8).
The produced flocs-like hydration products in M4 (Fig. 13 (c))
had a denser and more compact microstructure with relatively
smaller pores in comparison with C and M1. The improved
microstructure was due to the synergistic combination of the filler
effect and the pozzolanic reaction caused by RHA. This conclusion
was strongly supported by a previous study which reported a less
porous microstructure upon the addition of RHA [61]. Moreover,
the formation of floc-like hydration products in concrete prepared
with RHA was also reported previously [7]. The SEM observations
corresponded well with the observed increase in flexural and com-
8
Construction and Building Materials 299 (2021) 123900
Fig. 12. XRD patterns of C, M1, and M4 at 28 d.
pressive strength of M4. Several previous studies also reported that
the presence of RHA in cement mortar and concrete improved the
microstructures due to its pozzolanic and filler effect by reducing
the CH and porosity [26,61].
3CaðOHÞ2 þ SiO2 ðRHAÞ
þ H2 OÒ3CaO:2SiO2 :3H2 O ðC  S  HÞ ð8Þ
3.9. TG-DTG
The results of TG-DTG analysis for the 28-d cured C, M1, and M4
are shown in Fig. 14. The initial mass losses in the range of 50 °C–
410 °C, 50 °C–420 °C and 50 °C–680 °C in C, M1, and M4 were
4.39%, 4.65%, and 7.68%, respectively. For C and M1, these mass
losses were mainly attributed to the loss of water from C-S-H
and ettringite. As for M4 (which had the most C-S-H, reflected by
S. Nasiru, L. Jiang, L. Yu et al. Construction and Building Materials 299 (2021) 123900

Fig. 13. SEM images of (a) C, (b) M1, and (c) M4.

the highest water loss of 7.68%), these mass losses were due to the
water loss from C-S-H. There was a slope in the TG curve of C
between 410 °C and 420 °C, which was attributed to the dehydra-
tion of CH [62]. The decomposition of CH in C occurred in the tem-
perature range of 420 °C–550 °C, resulting in a 1.1% weight loss. In
M1, the dehydration and decomposition of CH occurred in the tem-
perature range of 420 °C–520 °C, resulting a weight loss of 5.94%. In
M4, however, no decomposition in this temperature range was
observed, indicating the absence of CH due to the depletion by
the RHA-induced pozzolanic reaction.

Fig. 14. TG/DTG of (a) C, (b) M1, and (c) M4..

9
S. Nasiru, L. Jiang, L. Yu et al.
Sharp endothermic peaks were observed in M1 (at 460°C) and M4
(at 700°C) due to the decarbonation reactions. This observation was
consistent with a previous study [63]. A less significant decarbona-
tion peak was also observed in C at 600 °C. Moreover, the decompo-
sition of CaCO3 into CaO and CO2 occurred in all the three samples.
The release of CO2 was observed at 714 °C for C, at 705 °C for M1,
and at 710 °C for M4, resulting in a corresponding weight loss of
4.54%, 4.24%, and 3.03%, respectively. This varying difference in
weight loss in the RHA containing specimen reflected a decrease in
CH due to the pozzolanic reaction. Previous studies also reported
that a decrease in CH led to the generation of hydration products
with a low calcium to silica ratio [64,65]. The TG-DTG findings cor-
responded well with the XRD and SEM observations. The low cal-
cium to silica ratio and the pozzolanic reaction combined to
effectively suppress the ASR expansion, as shown in Section 3.6 [66].
4. Conclusions
Based on the findings from this study, the following conclusions
can be drawn:
1. A partial replacement (50%) of sand by RG led to a decrease in
both flexural and compressive strength at all curing ages. The
addition of RHA in the RG incorporated samples improved both
flexural and compressive strength at 28 d of curing, with the
optimal strength obtained in the sample with replacing 30%
cement by RHA.
2. The chloride penetration resistance of the RHA incorporated
samples was significantly improved. The 30% RHA incorporated
sample showed the smallest penetration depth (0.9 mm), as
well as the smallest value of non-steady-state mitigation coef-
ficient (D = 0.10  10-12 m2/s).
3. The addition of RHA as a replacement of cement in the RG incor-
porated samples effectively suppressed the ASR expansion
caused by reaction between the reactive silica from RG and
the alkali from cement. All the RHA incorporated samples
showed an ASR expansion far below the permissible limit indi-
cated by the ASTM C1260.
4. The micro filler effect of RHA and the formation of more sec-
ondary C-S-H gels at the expense of CH through the RHA-
induced pozzolanic reaction combined to contribute to the
observed improvements in the mechanic properties and durabil-
ity of the RHA incorporated samples. The absence of CH in the
RHA containing samples (due to the pozzolanic reaction) was fur-
ther substantiated by the results of XRD, SEM, and TG analysis.
CRediT authorship contribution statement
Salifu Nasiru: Investigation, Methodology, Writing - original
draft. Linhua Jiang: Supervision, Writing - review & editing. Lin
Yu: Visualization, Data curation. Hongqiang Chu: Formal analysis.
Yu Huang: Writing - review & editing. Chun Pei: Formal analysis.
Yue Gu: Visualization. Weizhun Jin: Methodology. Edwin Eyram
Klu: Visualization. Ming-Zhi Guo: Conceptualization, 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.
10
Construction and Building Materials 299 (2021) 123900
Acknowledgement
The authors would like to acknowledge the financial support of
the National Key Research and Development Program of China
(2016YFA0203000), the Fundamental Research Funds for the Cen-
tral Universities (No. 2019B16614), the National Natural Science
Foundation of China (No. 52078183), Opening Research Fund of
State Key Laboratory of Geomechanics and Geotechnical Engineer-
ing, Institute of Rock and Soil Mechanics, Chinese Academy of
Sciences (Grand No. Z020012), and Opening Project of Shenzhen
Durability Centre for Civil Engineering, Shenzhen University
(GDDCE17-8).
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