materials
Article
Combined Freeze-Thaw and Chloride Attack Resistance of
Concrete Made with Recycled Brick-Concrete Aggregate
Yao Yu 1 , Jian Wang 1 , Ninghui Wang 1 , Chenjie Wu 1 , Xiaojing Zhang 1 , Dezhi Wang 1,2,3, *






Citation: Yu, Y.; Wang, J.; Wang, N.;
Wu, C.; Zhang, X.; Wang, D.; Ma, Z.
Combined Freeze-Thaw and Chloride
Attack Resistance of Concrete Made
with Recycled Brick-Concrete
Aggregate. Materials 2021, 14, 7267.
https://doi.org/10.3390/ma14237267
Academic Editor: Dolores Eliche
Quesada
Received: 18 October 2021
Accepted: 25 November 2021
Published: 28 November 2021
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with regard to jurisdictional claims in
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iations.
Copyright: © 2021 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Materials 2021, 14, 7267. https://doi.org/10.3390/ma14237267
and Zhipeng Ma 1
1 School of Civil & Water Conservancy Engineering, Ningxia University, Yinchuan 750021, China;
yuyao2021@nxu.edu.cn (Y.Y.); wangjian2021@nxu.edu.cn (J.W.); wangninghui2021@nxu.edu.cn (N.W.);
wuchenjie2021@nxu.edu.cn (C.W.); zhangxiaojing2021@nxu.edu.cn (X.Z.); mazhipeng2021@nxu.edu (Z.M.)
2 Ningxia Water-Efficient Irrigation Engineering Research Center, Yinchuan 750021, China
3 Water Resources Engineering Research Center in Modern Agriculture in Arid Regions,
Yinchuan 750021, China
* Correspondence: wangdzh@nxu.edu.cn
Abstract: The objective of this study was to investigate the physico-chemical properties of concrete
made with recycled brick-concrete aggregate, which was the mixture from waste concrete and waste
clay brick in a 7:3 ratio. Specifically, this paper investigated the mechanical properties, freeze-thaw
resistance, and distribution of water-soluble chloride ions of concrete containing RBCA and fly
ash (FA) against combined freeze-thaw and sodium chloride attack. Concrete containing RBCA
replacement of natural coarse aggregate and fly ash replacement of Portland cement was subjected to
45 freeze-thaw cycles containing sodium chloride solution. It was discovered that the mechanical
properties and freeze-thaw resistance to sodium chloride attack gradually decreased with increasing
RBCA content. At the same time, a replacement level of 15% FA by weight resulted in significant
improvements in compressive strength and resistance to combined freeze-thaw and chloride attack.
Furthermore, using a replacement of 30% FA by weight markedly improved the resistance to chloride
ion penetration of concrete due to the lowest water-soluble chloride content.
Keywords: recycled aggregates; fly ash; corrosion; water-soluble chloride content; freeze-thaw
1. Introduction
As industrial growth and urbanization continue, the cumulative amount of construc-
tion solid waste grows rapidly. In the last five years, the utilization rate of construction
solid waste in Japan, the Netherlands, Germany, and Denmark has reached 80% or more,
whereas, in China, the utilization rate is only around 47.7% [1]. As a result, improving
the replacement rate of recycled aggregate and the performance of concrete has become a
critical research area to enhance the recycling process of recycled aggregate. At present,
the majority of the recycled aggregate utilized domestically in China and internationally is
made from waste concrete after crushing, sorting, and screening. Actually, clay brick which
is the main material of masonry structures, accounts for a significant portion of building
and demolition waste. If broken bricks were widely employed in concrete manufactur-
ing, the shortage of natural sand and stone resources would be alleviated, the recovery
efficiency of building solid waste would be increased [2,3].
In general, recycled aggregate degrades the performance of concrete, as demonstrated
by a significant number of scholars [4–7]. The quality of recycled concrete was depended on
many factors, including the strength of parent concrete of recycled concrete aggregate (RCA)
and the proportion of RCA [8]. Typically, for RCA with higher strength of parent concretes
(PC), a lower replacement rate was conducive to the strength of recycled concrete. Kou [9]
prepared concrete with RCA derived from multiple PC, including 30, 45, 80, and 100 MPa.
The tests indicated that the mechanical properties of the recycled concrete derived from PC
of 30 and 45 MPa were fallen 21.1% and 12.6%, while concrete with RAC from another two
https://www.mdpi.com/journal/materials
Materials 2021, 14, 7267 2 of 15

PC and natural aggregate presented almost the same. Statistical analyses by Ohemeng [10]
concluded that recycled aggregate would be unfavorable to the performance of concrete
when PC was lower than 50 MPa. As the proportion of RCA increased, the performance of
concrete was worse due to amplified porosity [11]. Moghadam [12] conducted mechanical
experiments on three concrete mixtures containing 0%, 50%, and 100% by weight of RCA
from three types of PC. When the strength of PC was 20, 40, and 80 MPa, the strength
ratios of concrete with 50% RCA and 100% RCA were 1.20, 1.11, and 1.08, respectively.
The results discovered that the mechanical properties presented a downward trend with
increasing RCA while elevating the PC strength of the RCAs can weaken the strength
loss rate. In other words, the replacement percentage of recycled aggregate was the main
indicator to dominate the mechanical properties of concrete while the strength of PC was
constant. Indeed, performance degradation of recycled concrete was due to the presence
of two additional interfacial transition zones (ITZ) with low particle density. One of them
existed between natural aggregate and old mortar adhered to the recycled aggregate, and
the other existed between natural mortar and old mortar [13,14]. The microstructure of
ITZ was observed by scanning electron microscope (SEM), the concentration of calcium
hydroxide crystal was higher, and the porosity was larger [15]. The porosity of the mortar
matrix is about 1/3 of the maximum porosity of ITZ [16]. As the residual old mortar
was difficult to be removed completely, the higher volume fraction of aggregate was, the
larger the weak area would be [17]; therefore, the replacement rate affected the macro
performance of concrete.
In real environments, structural failure is not only caused by inadequate strength but
also caused by a combination between mechanical and durability of deleterious issues.
Concrete durability was adversely influenced by many physical effects, including wear
of frictional surface, cracking on account of pore solution crystallization, faced with the
atrocious circumstance in temperature (frost or heat action, for instance), and detrimental
chemical effects, including lixiviating of the cement paste because of acidic solutions [18]
and expansive substances by sulfate attack [19,20]. In comparison, corrosion of reinforce-
ment by the chlorine ion in concrete structures [21] was one of the biggest and the most
serious factors in saline-alkali soil, areas covered with deicing salts, and coastal environ-
ments. Under the combination of chlorine corrosion and the freeze-thaw cycle, a more
complex physical and chemical process occurs where high free chloride ions would par-
tially destroy the passive film of reinforcement, and then the iron matrix would be exposed.
The corrosive battery was formed due to the potential difference between iron and passive
film. More severely, the temperature fluctuation further speeds up chloride diffusion. The
deterioration rate of concrete is controlled by the migration of water in concrete. On this
account, the parameter that the influence of the permeability of concrete on durability
should be evaluated. Fly ash, as an industrial by-product, was widely used to improve
concrete performance by virtue of its value attributes such as micro-aggregate filling and
pozzolanic effect [22,23]. The micro-aggregate filling effect reduced porosity and the poz-
zolanic effect consumed Ca(OH)2 , and then ITZ is enhanced. Finally, concrete performance
was enhanced wholly because the permeability of the constituent materials determined
the permeability of concrete. Kou et al. [24] stated that fly ash in proper proportion could
improve the frost resistance of recycled concrete and enhance its chloride penetration resis-
tance to some extent. They tested recycled concrete with 0, 25%, and 35% Class F fly ash and
pointed out that incorporating 25–35% fly ash was a practical way to improve the chloride
permeability resistance at the water-binder ratio of 0.45 and 0.55, which minimized the
total charge passed of recycled concrete at 28 and 90 days. Moreover, Kurda [25] extracted
the results of 655 concrete incorporating coarse RCA and FA, at least 28 days, from many
papers. It was found that the concrete with 20% fly ash exhibited a better performance
compared to the benchmark concrete. Other researchers [26,27] also confirmed through
tests such as the RCM and electric quantity methods that fly ash can improve concrete
impermeability, but higher levels of fly ash incorporation can be detrimental to chloride
penetration resistance of recycled concrete as a result of leading to higher porosity.
Materials 2021, 14, 7267 3 of 15

A good deal of research on the mechanical properties and durability of concrete made
with waste concrete aggregates may exist. However, research regarding the deterioration of
concrete composed of recycled brick-concrete aggregate (RBCA) is limited in the literature
and mainly focuses on the mechanical properties [28–31]. Generally, the crushed clay brick
aggregate absorbs more water than nature aggregate or recycled concrete aggregate, and
its porosity and crushing index are significantly greater. Poon [14] mixed recycled brick
aggregate and recycled concrete aggregate together, and the test results indicated that the
maximum dry density was lesser and the optimum moisture content larger than RCA
solely. Similarly, the mechanical properties of recycled concretes containing brick were also
affected by the replacement rate. Boukour manufactured mortars with 2.5%, 5%, 7.5%, and
10% brick waste of natural coarse aggregate, and there was a gradual downward trend
in the 28 days compressive and flexural strengths [32]. However, in terms of durability,
there were two opposite effects of aggregate size and volume fraction on the migration
coefficient of chloride ions. The positive effects included dilution and deformation effect,
which reduced the migration coefficient, and the negative effects included transition zone
and seepage, which increased the value [16]. The aggregate size and porosity are easy
to measure. However, when the shape of concrete aggregate inclusion is not standard,
the information of chloride ion migration coefficient in the interface transition zone is
very little, and it is difficult to test the interface transition zone alone. Lutz [33] estimated
the effective macroscopic conductivity of the medium by the Maxwell homogenization
method, which calculated the effective conductivity from a single-inclusion problem, and
verified that the conductivity decreased due to non-conductive inclusions while increased
due to ITZ. Until now, it has been difficult to unite the physical markers of recycled brick,
and dispersion in the findings persists. While there have been some advancements in the
mechanical properties of recycled brick-concrete aggregate (RBCA) concrete, there is a
gap in the knowledge needed to evaluate the durability of RBCA concrete. Given the vast
number of discarded bricks in construction solid waste, there is significant potential for
study into the performance of recycled concrete using RBCA.
As a result, in this study, the recycled brick–concrete aggregate (RBCA) was made
from waste concrete and waste clay bricks in a ratio of 7:3. Mechanical properties and
durability (frost resistance and permeability) of concrete with RBCA were investigated,
and the influence of RBCA and FA under the combined action of cyclic freeze-thaw and
chloride attack. Furthermore, the phase compositions of recycled concrete were determined
using microscopy and X-ray diffraction.

2. Experimental Program
2.1. Experimental Materials
2.1.1. Cement
An amount of 42.5R Ordinary Portland cement (OPC), in conformity with Chinese
standard GB175-2007 [34], which resemblance to EN197-1:2009, was used to make concrete
specimens. The composition and physical properties of OPC are illustrated in Table 1.

Table 1. Composition and physical properties of OPC.

Specific Initial Final

Al2 O3 Fe2 O3 CaO MgO SO3 Surface Setting Setting
SiO2 (%) Soundness
(%) (%) (%) (%) (%) Area Time Time
(m2 /kg) (min) (min)
14.1 5.19 2.17 43.5 5.00 2.93 348 195 255 qualified

2.1.2. Natural Aggregates

Classification of particle size was based on standard ASTM C125. Washed river sand
in the range of 4.75 mm (No. 4) and 0.15 mm (No. 100) was used as the fine aggregate.
 2.1.3. Recycled Aggregates
After removing steel reinforcement bars from waste concrete f
crushed in a jaw crusher, screened, and washed to obtain a continuo
Materials 2021, 14, 7267 4 of 15
4.75–31.5 mm, and finally mixed with recycled brick aggregate at a 7
sive strength of parent concretes was 40.7 MPa. In this study, the
1
wasCrushed
named RBCA,
limestone in theand
range recycled
of 31.5 mm (1concrete
4 in.) and 4.75aggregate
mm (No. 4) was and
usedrecycled
as the b
coarse aggregate.
was named RCA and RBA; RBAC, RAC, and RBA had the same par
ical2.1.3. Recycled Aggregates
characteristics test methods in accordance with Chinese stand
After removing steel reinforcement bars from waste concrete floor slabs, they were
Table
crushed2 and Figure
in a jaw 1 present
crusher, screened, the physical
and washed properties
to obtain a continuous grainand the grad
size range
of 4.75–31.5 respectively.
aggregate, mm, and finally mixed with recycled brick
Additionally, the aggregate
crushing at avalue
7:3 ratio.index
The of R
compressive strength of parent concretes was 40.7 MPa. In this study, the compound
theaggregate
resultswas were
namedclassified as type
RBCA, and recycled III according
concrete to Chinese
aggregate and recycled standard G
brick aggregate
solely was named RCA and RBA; RBAC, RAC, and RBA had the same particle gradation.
Physical characteristics test methods in accordance with Chinese standard JGJ 52-2006 [35].
Table
Table2.2 Physical
and Figure characteristics
1 present the physicalof recycled aggregates.
properties and the grading chart of recycled
aggregate, respectively. Additionally, the crushing value index of RBCA was 20.3%, and
Water to Chinese standard
the results were classified as type III according Apparent
GB/T 25177-2010 [36].
Proportion Bulk Den
No. Aggregate Sources Table 2. Physical characteristicsAbsorption
of recycled aggregates. Density
(%) (kg/m3
Water (%) Apparent (kg/m3) Crushing
Aggregate Proportion Bulk Density
No. Absorption Density Value Index
WasteSources
concrete (%) 70 (%) 3 (kg/m3 )
RBCA 12.8(kg/m ) 2302 (%)
1020
Waste brick
Waste concrete 70 30 12.8 2302 1020 20.3
RBCA
Waste brick 30
RCA Waste concrete 100 6.1 2409 1120
RCA Waste concrete 100 6.1 2409 1120 15.9
RBA RBA Waste brick
Waste brick 100 100 18.0 18.0 2051 858 2051 25.5 858

100

80
Percent Passing

60

40

20

0
0.01 0.1 1 4.75 10 31.5 100
sieves size (mm)
Figure 1. Grading chart of recycled aggregate.
Figure 1. Grading chart of recycled aggregate.
2.1.4. Other Materials
The polycarboxylate superplasticizer was used in the concrete mixtures to maintain the
2.1.4. Other Materials
concrete slump of 90–100 mm, and the slump loss in one hour was 40–50 mm. Anhydrous
sodium
Thechloride with 99.5% puritysuperplasticizer
polycarboxylate provided the raw material
was for chloride
used in solutions. The
the concrete
Class F fly ash (FA) was used as supplementary cementitious material.
the concrete slump of 90–100 mm, and the slump loss in one hour w
drous sodium chloride with 99.5% purity provided the raw mater
tions. The Class F fly ash (FA) was used as supplementary cementiti
Materials 2021, 14, 7267 5 of 15

2.2. Mix Proportion

Concrete was manufactured with a water-binder ratio of 0.4, the binder material of
450 kg/m3 , and a sand ratio of 0.34. There were two different percentages of RBCA (i.e., 80
and 100 wt.% of natural coarse aggregates). The RBCA was made of waste concrete and
waste clay bricks in a ratio of 7:3. There were three different percentages of FA (i.e., 0, 15,
and 30 wt.% of OPC). The actual concrete mix proportions are exhibited in Table 3.

Table 3. Mix proportions of recycled concretes (kg/m3 ).

Coarse Aggregate Binding Material

No. Natural Sand Water
RBCA Natural Gravel OPC FA
R100-FA0 1201 0 619 450.0 0 180
R100-FA15 1201 0 619 382.5 67.5 180
R100-FA30 1201 0 619 315.0 135 180
R80-FA0 960.8 240.2 619 450.0 0 180
R80-FA15 960.8 240.2 619 382.5 67.5 180
R80-FA30 960.8 240.2 619 315.0 135 180

2.3. Experimental Methods

The preparation process of specimens complied with the standard ASMT C192. Add
coarse aggregate, partial water, and the solution of the polycarboxylate superplasticizer
into the mixer. Then, start the mixer and add cementitious material, fine aggregate, and
remaining water. Mix in the mixer for 3 min, rest for 3 min, and mix for another 2 min to
mix them evenly. Prismatic specimens 100 mm × 100 mm × 400 mm and cube specimens
100 mm in size were cast in plastic molds, removed after about 24 h, and cured for 28 days at
20 ± 2 ◦ C with a relative humidity of at least 95%. Prismatic specimens were used to assess
frost resistance, while cube specimens tested compressive strength. Axial compressive
strength tests were performed in conformity to ASMT C39, and test results were determined
to be the mean values of every 3 specimens.

2.3.1. Freeze-Thaw Cycles in NaCl Solution

The rapid freeze-thaw process was in accordance with ASTM C666. Prismatic spec-
imens of 100 mm × 100 mm × 400 mm were cured for 28 days before being immersed
at 1 mm depth in water for 7 days. Five surfaces were sealed with epoxy resin glue
(except for one side of 100 × 400 mm2 ) to ensure chlorine penetrates from the reserved
erosion surface when immersed in saline solution (Figure 2a). A total of 45 freeze-thaw
cycles were performed, with each cycle lasting 6 h (3 h frozen at −18 ± 2 ◦ C, and 3 h
thawing at 5 ± 2 ◦ C). Mass and transverse frequency were determined for specimens
after 15 and 45 freeze-thaw cycles using an electronic scale and a dynamic elastic modulus
measurement instrument (Figure 3), respectively. The mass-loss rate (MLR) and the relative
dynamic elastic modulus (RDEM) were calculated via Equations (1) and (2).

m0 − m n
MLR = × 100 (1)
m0

f n2
RDEM = × 100 (2)
f 02
where MLR is the mass loss rate (%); m0 is the initial mass (g); mn is the mass of a concrete
prismatic specimen that underwent n freeze-thaw cycles (g). RDEM in % is the relative
dynamic elastic modulus of concrete; f 0 is the initial transverse frequency (Hz); fn is
the transverse frequency of a prismatic concrete specimen that underwent n freeze-thaw
cycles (Hz).
Materials 2021, 14, 7267

Materials2021,
Materials 14,7267
2021,14, 7267 66of
of16
15

(a) (b)
(a) (b)
Figure 2. Schematic
Figure
Figure2.2.Schematic
diagram
Schematicdiagram
diagramof
ofsampling
sampling
ofsampling for for water-soluble
forwater-soluble
water-solublechloride
chloride
chloridecontent
content
contenttest.
test.(a)
test. (a)ofSchematic
(a)Schematic
Schematicof test
testblock
ofsalt-freeze
blockfor
test block for salt-fre
forsalt-freeze
test.test.
(b) Cross-section
test.(b)
(b)Cross-section view
Cross-sectionview of
viewof stratified
ofstratified sampling.
stratifiedsampling.
sampling.

Figure 3. DT-20 Dynamic Elastic Modulus Measurement instrument.

2.3.2. Water-Soluble Chloride Test

Figure
Figure 3.3.DT-20
Drilled DT-20
concreteDynamic
Dynamic Elastic
vertically
Elastic inward
Modulus Modulus
along the
Measurement Measurement
erosion surface
instrument. instrument.
by layer as described in
Test method ASTM C42 and collected concrete powder samples. Referring to ACI 318, the
2.3.2. Water-Soluble
concrete protective layerChloride Test is concentrated in 10–50 mm; it is 75 mm only in rare
thickness
2.3.2. Water-Soluble Chloride Test
cases.Drilled concrete
Therefore, vertically
the chloride ioninward along the
concentration waserosion
focusedsurface
on inby thelayer
rangeas of
described
0–50 mm in
Drilled
Test method
from the concrete
ASTM
erosion C42 and
surface. vertically inwardpowder
collected concrete along the erosion
samples. surface
Referring by318,
to ACI layer theas desc
Test method
concrete
The sampling ASTM
protective layerC42
diagram isand
thickness collected
depictedis concentrated
in Figureconcrete
2b,inand powder
10–50themm; itsamples. Referring
is 75 mmchloride
water-soluble only rare to ACI
in test
cases. Therefore, the chloride ion concentration was focused
concrete protective layer thickness is concentrated in 10–50 mm; it is 75 mm only
procedure was in accordance with ASTM C1218 (as shown on
in in
Figurethe range
4). of
Samples0–50 mm
were
from the
soaked
cases. in erosion
distilledsurface.
Therefore, water
the and stood for
chloride ion24concentration
h after vibrating wasfor 5focused
min to extracton in chloride
the range of 0
The sampling
ions. Then 2 drops of diagram is depictedwere
phenolphthalein in Figure
used 2b,as aandcolortheindicator,
water-solubleand itchloride
turned red test
from the erosion
procedure was in
surface. with ASTM C1218 (as shown in Figure 4). Samples were
accordance
because the aqueous solution was alkaline. Subsequently, dilute sulfuric acid was added
soaked
until The
the in sampling
distilled
solution water
was diagram
and stood
colorless. is
fordepicted
In the 24 h 10
end, after in Figure
vibrating
drops of K2CrOfor 2b, and
54 solution
min the
werewater-soluble
to extract chloride
an indicatorions. chlor
procedure
Then
added 2todrops
recordwas
of the in accordance
phenolphthalein
consumption were
of with
AgNOused3 ASTM
as a color
when C1218
peach indicator, (asand
precipitation shown in red
itformed.
turned Figure
Thebecause
chem- 4). Sampl
the
ical aqueous
soaked solution
in distilled
reactions was
are shownwater alkaline. Subsequently,
and stood
in Equations (3) and for dilute sulfuric
(4),24respectively.
h after vibrating acid was
The silverfor added
ion5ofminuntil
AgNO the
to 3extract c
solutionreacted
solution was colorless. Inchloride
the end,ion 10 drops of silver
K2 CrOchloride,
4 solution were anexcess
indicator added
ions. Then 2 drops of phenolphthalein were used as a color indicator,ion
with the to form and then silver and it tur
to record with
interacted the consumption
chromate ionof of AgNO when peach
K2CrO34 solution to formprecipitation formed. The
peach precipitation. chemical
Chloride ion
because
reactions the aqueous
aremeasured solution
shown in Equations was
(3) and alkaline.
(4), respectively. Subsequently,
TheAgNO silver 3ion dilute
of AgNO sulfuric
3 solution
acid wa
content was by recording the consumption of the solution. The water-
until
reactedthe
soluble solution
with thecontent
chloride was
chloride colorless.
ion
(WSCC) to form In the
silver
was calculated end,
chloride, 10
and drops
via Equation then(5). of K2CrO
excess solution
silver4 ion interactedwere an in
with
added chromate
to recordion of K2consumption
the CrO4 solution toof form
AgNO peach precipitation.
3 when peach Chloride
precipitationion content
formed. Th
was measured by recording the 𝐴𝑔 + 𝐶𝑙 →
consumption of 𝐴𝑔𝐶𝑙
the ↓
AgNO solution. The water-soluble (3)
ical reactions are shown in Equations (3) and (4), respectively. The silver ion of 3
chloride content (WSCC) was calculated via Equation (5).
solution reacted with the chloride 2𝐴𝑔 + 𝐶𝑟𝑂 ion → to𝐴𝑔 form𝐶𝑟𝑂silver
↓ chloride, and then(4)excess si
−
interacted with chromate ionAgof+CK CrO
+2Cl V→4 solution
× AgCl ↓ to form peach precipitation.
0.03545 (3) Chlo
𝑊𝑆𝐶𝐶 = × 100 (5)
content was measured by recording the V′
consumption of the AgNO 3 solution. The
2Ag+ + CrO42 −G →
× Ag2 CrO4 ↓
V (4)
soluble chloride content (WSCC) was calculated via Equation (5).
𝐴𝑔 + 𝐶𝑙 → 𝐴𝑔𝐶𝑙 ↓
2𝐴𝑔 + 𝐶𝑟𝑂 → 𝐴𝑔 𝐶𝑟𝑂 ↓
Materials 2021, 14, 7267 7 of 1

Materials 2021, 14, 7267 where WSCC is the water-soluble chloride content of concrete (%); CAgNO3 in70.02
of 15 mol/L
the concentration of AgNO3 prepared; V is the AgNO3′s consumption of titrations (mL
V’ is the amount of distilled water was used to dissolve the powdery sample.
 
Materials 2021, 14, 7267 CAgNO3 V × 0.03545 7 of 16
WSCC = V0
× 100 (5)
G× V

whereWSCC
where WSCCisisthe
thewater-soluble
water-solublechloride
chloridecontent ofof
content concrete (%);
concrete CAgNO3
(%); CAgNO3inin0.02
0.02mol/L
mol/Lisis
the
the concentration of AgNO33 prepared; V is the AgNO33′s consumption of titrations (mL);
concentration of AgNO prepared; V is the AgNO ’s consumption of titrations (mL);
0 is the amount of distilled water was used to dissolve the powdery sample.
VV’ is the amount of distilled water was used to dissolve the powdery sample.

Figure 4. Schematic diagram of the procedure for water-soluble chloride content test.

3. Results and Discussion

3.1.Figure
Compressive Strength
Figure4.4.Schematic
Schematicdiagram
ofofRecycled
diagramof
Concrete
theprocedure
the procedurefor
forwater-soluble
water-solublechloride
chloridecontent
contenttest.
test.
3.1.1. Compressive Strength and RBCA Content
3.
3. Results
Results and
and Discussion
Discussion
The compressive
3.1. Compressive Strength strength of concrete
of Recycled Concrete with different recycled aggregate content at 2
3.1. Compressive Strength of Recycled Concrete
days depicted
3.1.1. in Figure
Compressive 5 shows
Strength that the
and RBCA R100 series concrete was weaker in compressio
Content
than3.1.1.
the Compressive
R80 series Strength and
concrete RBCA
across
The compressive strength of concrete with all Content
fly ashdifferent
contents. Whenaggregate
recycled the content of RBCA
content at wa
increased The compressive
from 80%
28 days depicted strength
to 100%,
in Figure of concrete
the compressive
5 shows with different
strength
that the R100 series recycled
of was
concrete aggregate
concrete
weaker with content at 28
0%, 15%, and 30%
in compression
daysthe
than depicted
R80 in Figure
series 5 shows
concrete acrossthat the
all flyR100
ash series concrete
contents. When was
the weaker
content in
ofcompression
RBCA was
of FA dropped by 2.60%, 7.28%, and 2.18%, respectively. The results indicated a negativ
than the R80
increased from series
80% concrete
to 100%, across
the all fly ashstrength
compressive contents.
of When
concretethewith
content
0%, of RBCA
15%, and was
30%
effect between the content of RBCA and mechanical properties that the 28-day compres
increased
of fromby
FA dropped 80% to 100%,
2.60%, 7.28%,theand
compressive strength ofThe
2.18%, respectively. concrete with
results 0%, 15%,
indicated and 30%
a negative
siveofstrength
FAbetween of concrete
dropped 2.60%,reduced
bycontent 7.28%, with
and an respectively.
2.18%, increase in RBCA Thethat replacement.
results
effect the of RBCA and mechanical properties the indicated a negative
28-day compressive
effect between the content of RBCA and mechanical
strength of concrete reduced with an increase in RBCA replacement. properties that the 28-day compres-
sive strength of concrete reduced with an increase in RBCA replacement.
50
FA0
FA15
compressive strength (MPa)

50
FA0FA30
FA15
compressive strength (MPa)

45.3 FA30
45
45.3
45
42.3 42
42.3 41.2 41.2 42
41.2 41.2 40.3
40 40.3
40

35 35
8080 100
100
RBCA replacement
RBCA replacement rate(%)
rate(%)
Figure 5. Twenty-eight-day compressive strength of concrete with different recycled aggregate content.
Figure 5. Twenty-eight-day compressive strength of concrete with different recycled aggregate
Figure 5. Twenty-eight-day compressive strength of concrete with different recycled aggregate
content.
content.
Some differences emerged, by comparison, the values of the R80 and R100 series in
Some5.differences
Figure emerged,
That R80 series concreteby
hadcomparison, the values
a margin of increase of the R80
of 2.2–7.9% than and
R100R100
seriesseries i
Figure 5. That
concrete R80
in the series
case of theconcrete
same mixhad a margin
proportion. of increase
Distinctly, of could
this gap 2.2–7.9% thantoR100
attribute the serie
concrete in the case of the same mix proportion. Distinctly, this gap could attribute to th
s 2021, 14, 7267

Materials 2021, 14, 7267 volume fraction of recycled aggregate. The extra added brick aggregate 8 ofoffered
15 a
effect of positive and negative superimposition. On the one hand, recycled brick ag
had a lower compressive strength and a higher crushing index than recycled conc
Some differences emerged, by comparison, the values of the R80 and R100 series in
gregate, so the compressive strength of the R100 series was reduced to some
Figure 5. That R80 series concrete had a margin of increase of 2.2–7.9% than R100 series
[30,31,37]. Oninthe
concrete theother
case ofhand,
the samethe brick
mix aggregate
proportion. had this
Distinctly, a high porosity
gap could andto water
attribute
tion capacity (18%), which was three times than RCA, allowing it to absorba an am
the volume fraction of recycled aggregate. The extra added brick aggregate offered
mixed effect of positive and negative superimposition. On the one hand, recycled brick
mixingaggregate
water from the mortar mixture early on and slowly release it later. Due
had a lower compressive strength and a higher crushing index than recycled
absorption and
concrete desorption
aggregate, so the properties of the brick
compressive strength of the aggregate,
R100 series wasit can act to
reduced assome
a source o
extent
water for the[30,31,37].
concrete On later.
the other hand, the aided
Moisture brick aggregate
in the had a highhydration
further porosity andof water
the ceme
absorption capacity (18%), which was three times than RCA, allowing it to absorb an
materials, ensuring homogeneous curing within the concrete mass and thus inc
amount of mixing water from the mortar mixture early on and slowly release it later.
the compressive strengthand
Due to the absorption of desorption
the mortar [38]. In
properties of addition, the actual
the brick aggregate, it canwater-binder
act as a
source of curing water for the concrete later. Moisture aided in
concrete with RBCA below the designed value results in strength was relatively hthe further hydration
of the cementitious materials, ensuring homogeneous curing within the concrete mass
and thus increasing the compressive strength of the mortar [38]. In addition, the actual
3.1.2. Compressive Strength
water-binder ratio of concreteand
with FA Content
RBCA below the designed value results in strength was
relatively high.
Trends on the strength curve of concrete with different mix ratios exhibited th
(Figure3.1.2.
6). When the content
Compressive of FA
Strength and increased from 0%, 15% to 30%, these curves w
FA Content
and then down.
Trends on Specifically, 15%
the strength curve of FA generated
concrete strength
with different growth
mix ratios bythearound
exhibited same 7%
(Figure 6). When the content of FA increased from 0%, 15% to 30%,
under R80 and R100 series, respectively. However, the strength for the concrete prthese curves went up
and then down. Specifically, 15% FA generated strength growth by around 7% and 2%
using 30%
under FA compared
R80 and torespectively.
R100 series, that of corresponding concrete
However, the strength no flyproduced
for the concrete ash had an a
shrinkage
usingof 2.4%.
30% This phenomenon
FA compared was attributed
to that of corresponding concrete noto fly
micro-aggregate
ash had an averagefilling
pozzolanic effects of fly ash [20,21]. Nevertheless, a high volumefilling
shrinkage of 2.4%. This phenomenon was attributed to micro-aggregate andash
of fly the incorp
pozzolanic effects of fly ash [20,21]. Nevertheless, a high volume of fly ash incorporation
magnified totaltotal
magnified porosity
porosityresult
result inindensity
density reduction.
reduction.

50 R80
R100
compressive strength (MPa)

45

40

35
0 15 30
FA replacement rate(%)

Figure 6. Twenty-eight-day compressive strength in different FA content.

Figure 6. Twenty-eight-day compressive strength in different FA content.
3.2. The Mass Loss Rate (MLR)
As shown in Figure 7, MLR of concrete specimens containing RBCA was performed
3.2. Theusing
Mass Loss Rate (MLR)
45 freeze-thaw cycles in a 3.0% by weight NaCl solution (3%NS-45FT).
As shownThe MLR increased7,asMLR
in Figure the number of freeze-thaw
of concrete cycles and
specimens the amountRBCA
containing of RBCA was per
in the concrete grew, and its value directly represented the extent of concrete spalling. In
using 45 freeze-thaw cycles in a 3.0% by weight NaCl solution (3%NS-45FT).
the case of R100, the MLR of concrete containing 0, 15%, and 30% FA had increased to
6.4%, 5.6%, and 6.2% of their initial value in the sequence, respectively, whereas in the case
 Materials 2021, 14, 7267 7.0 FA0 9 of 15
FA15
FA30
6.5 6.4
terials 2021, 14, 7267 of R80, the counterpart values were 6%, 5.1%, and
6.2 5.7%, respectively. According to the
results, 15% FA6reduced MLR to a minimum of 5.1% after 45 freeze-thaw cycles in a 3.0%
6.0

MLR (%)
NaCl solution. Additionally, the MLR of concrete without FA was somewhat greater than
5.7
concrete containing 30% FA.
5.6
5.5

7.0 5.1 FA0

5.0 FA15
FA30
6.5 6.4
4.5
80 100 6.2
6 RBCA replacement rate(%)
MLR (%)

6.0
5.7the mass loss rate of 3%NS-45FT.
Figure 7. Multifactor influence on
5.6
5.5
The MLR increased as the number of freeze-thaw cycles and the amount of RBCA in
the concrete grew, and5.1
its value directly represented the extent of concrete spalling. In the
case of 5.0
R100, the MLR of concrete containing 0, 15%, and 30% FA had increased to 6.4%,
5.6%, and 6.2% of their initial value in the sequence, respectively, whereas in the case of
R80, the counterpart values were 6%, 5.1%, and 5.7%, respectively. According to the re-
sults, 15%
4.5 FA reduced MLR to a minimum of 5.1% after 45 freeze-thaw cycles in a 3.0%
80
NaCl solution. Additionally, 100without FA was somewhat greater than
the MLR of concrete
concrete containing 30% FA.
RBCA replacement rate(%)
3.3. The 7.Relative
Figure Dynamic
Multifactor Elastic
influence on theModulus
mass loss (RDEM)
rate of 3%NS-45FT.
Figure 7. Multifactor influence on the mass loss rate of 3%NS-45FT.
3.3.Figure 8 illustrates
The Relative the decline
Dynamic Elastic Modulusin (RDEM)
RDEM of concrete specimens exposed to 3% NS-
45FT. All RDEMs
Figure exhibited
8 illustrates a declining
the decline in RDEM trend, and their
of concrete amplitudes
specimens ranged
exposed toand from 9.58% to
3% NS-45FT.
46.92
The MLR
% of their
increased
starting
as the number
value.trend,
Furthermore,
of freeze-thaw
R100-FA0ranged
had the
cycles the amount
All RDEMs exhibited a declining and their amplitudes fromgreatest reduction in
9.58% to 46.92%
the concrete
RDEM,
of theirwith agrew,
starting
and its
noticeably value
steep
value. Furthermore,curvedirectly
and a had
R100-FA0
represented
total RDEM
the
the extent
decrement
greatest reduction of
of concrete
53.08
in RDEM, %, spa
followed
with
case of R100,steep
bya R100-FA15
noticeably the curve
and MLRand ofaconcrete
R80-FA15. total RDEMcontaining
decrement of0, 15%,followed
53.08%, and 30% FA had increas
by R100-FA15
and R80-FA15.
5.6%, and 6.2% of their initial value in the sequence, respectively, whereas in
100
R80, the counterpart values were 100
6%, 5.1%, and 5.7%, respectively. Accordin
98
sults, 15% FA reduced MLR to98a minimum of 5.1% after 45 freeze-thaw cycle
96 NaCl solution. Additionally, the96 MLR of concrete without FA was somewhat g
94 concrete containing 30% FA. 94
RDEM(%)

RDEM(%)

92 92
R100-FA0
90 3.3. The Relative Dynamic Elastic90Modulus (RDEM)
R100-FA15
R100-FA30
88 R80-FA0 88
R80-FA15
Figure 8 illustrates the decline inR100-FA0
RDEM of concrete specimens exposed
86 86
R80-FA0
84
45FT. All RDEMs exhibited a declining
R80-FA30
84
trend, and their amplitudes ranged fro
0 15 45 0
46.92 % of their starting value. Furthermore, 15 R100-FA0 45had the greatest r
Number of freeze-thaw cycles Number of freeze-thaw cycles
RDEM, with a noticeably steep curve and a total RDEM decrement of 53.08 %
(a) (b)
by R100-FA15 and R80-FA15.
Figure 8. Cont.

100 100

98 98

96 96

94 94
RDEM(%)

RDEM(%)

92 92
R100-FA0
90 R100-FA15 90
Materials 2021, 14, 7267 10 of 16
Materials 2021, 14, 7267 10 of 15

100 100

98 98

96 96

94 94
RDEM(%)

RDEM(%)
92 92

90 90

88 88
R100-FA15 R100-FA30
86 R80-FA15 86 R80-FA30
84 84
0 15 45 0 15 45
Number of freeze-thaw cycles Number of freeze-thaw cycles

(c) (d)

100 100

98 98

96 96

94 94
RDEM(%)

RDEM(%)

92 92

90 90

88 R100-FA0 88 R80-FA0
R100-FA15 R80-FA15
86 R100-FA30 86 R80-FA30
84 84
0 15 45 0 15 45
Number of freeze-thaw cycles Number of freeze-thaw cycles

(e) (f)
Figure 8. The
Figure RDEM
8. The RDEM of of
concrete
concreteexposed to 3%NS-45FT.
exposed to 3%NS-45FT. (a)(a)
All,All,
(b) (b)
FA0,FA0, (c) FA15,
(c) FA15, (d) FA30,
(d) FA30, (e)(f)R100,
(e) R100, R80. (f) R80.
Note: R isNote—R
for is
for recycled brick-concrete aggregate; FA is for fly ash; numbers are the value of replacement
recycled brick-concrete aggregate; FA is for fly ash; numbers are the value of replacement rate (%). rate (%).

InInthe
theinstance
instance of
of the
theR100
R100series, RDEM
series, RDEM grew as fly
grew as ash
fly content increased,
ash content while the
increased, while the
R80 series curves pattern remained consistent. The vertical distance betweencurves
R80 series curves pattern remained consistent. The vertical distance between two two curves
in concrete without FA (Figure 8b) shows that the RDEM of the concrete was the most
in concrete without FA (Figure 8b) shows that the RDEM of the concrete was the most
responsive to RBCA concentration. In the case of concrete containing 30% FA (Figure 8d),
responsive to RBCA
the R100 series had aconcentration.
higher RDEM value In thethan
casethe
of concrete
R80 series,containing
which was30% FA (Figure
in contrast to 8d),
the
the behavior of concrete without FA or with 15% FA. As a result, a replacement level of to the
R100 series had a higher RDEM value than the R80 series, which was in contrast
behavior
15–30% FA of was
concrete without
favorable FA
to the or withof15%
resilience FA. As
concrete a result,
subjected to athe
replacement level of 15–
combined freeze-
30%
thawFAandwassaltfavorable
chloride to the resilience
solution of concrete subjected
attack. Furthermore, the RDEMto the of
value combined
concrete freeze-thaw
made
with
and varying
salt RBCA
chloride content attack.
solution performs differently depending
Furthermore, the RDEM on the
valueamount of FA. made with
of concrete
varying RBCA content performs differently depending on the amount of FA.
3.4. Water-Soluble Chloride Content (WSCC)
3.4.1. WSCC and RBCA Content
3.4. Water-Soluble Chloride Content (WSCC)
Figures 9 and 10 show the WSCC of concrete samples subjected to 3% NS-45FT. The
3.4.1.
WSCC WSCC and RBCA
of specimens Content
showed a downward trend with increasing distance from the erosion
surface, stabilizing
Figures 9 and 10at ashow
depththe
of 30–40
WSCC mm, as shown samples
of concrete in Figure subjected
9. Even with
to the
3% variable
NS-45FT. The
FA content,
WSCC the WSCC
of specimens of the R100
showed series wastrend
a downward typically
withgreater than the
increasing R80 series
distance from forthe
theerosion
same depth. The WSCC curve for concrete with a varied amount of RBCA (i.e.,
surface, stabilizing at a depth of 30–40 mm, as shown in Figure 9. Even with the variable 80 and
100 wt.%) displayed a more significant divergence when concrete contained 15% FA.
FA content, the WSCC of the R100 series was typically greater than the R80 series for the
same depth. The WSCC curve for concrete with a varied amount of RBCA (i.e., 80 and 100
wt.%) displayed a more significant divergence when concrete contained 15% FA.
 Materials 2021, 14, 7267 11 of 16
Materials 2021, 14, 7267 11 of 16
Materials 2021, 14, 7267 11 of 15

0.9
R100-FA0
0.9
0.8 R100-FA15
R100-FA0
0.8 R100-FA30
R100-FA15
0.7
R80-FA15
R100-FA30
0.7
0.6 R80-FA30
R80-FA15

WSCC(%)
0.6
0.5 R80-FA30
WSCC(%) 0.5
0.4
0.4
0.3
0.3
0.2
0.2
0.1
0.1
0.0
0.0 0 10 20 30 40 50
0 10 20depth(mm)
30 40 50
depth(mm)
Figure 9. WSCC of concrete samples after 3%NS-45FT.
Figure
Figure 9. WSCC
9. WSCC of concrete
of concrete samplesafter
samples after3%NS-45FT.
3%NS-45FT.

0.9 0.9
R100-FA15 R100-FA30
0.90.8 R80-FA15 0.90.8 R80-FA30
R100-FA15 R100-FA30
0.80.7 R80-FA15
0.80.7 R80-FA30
0.70.6 0.70.6
WSCC(%)
WSCC(%)

0.60.5 0.60.5
WSCC(%)
WSCC(%)

0.50.4 0.50.4
0.40.3 0.40.3
0.30.2 0.30.2
0.20.1 0.20.1
0.10.0 0.10.0
0 10 20 30 40 50 0 10 20 30 40 50
0.0 depth(mm) 0.0
0 10 20 30 40 50 0 10 20 depth(mm)
30 40 50
depth(mm) depth(mm)
(a) (b)
Figure 10. Influence of aggregate replacement rate on WSCC. (a) FA15,(b)
(a) (b) FA30. Note-FA is for fly
Figure 10. Influence of aggregate replacement rate on WSCC. (a) FA15, (b) FA30. Note: FA is for fly
ash;
Figure numbers
ash;10. are
arethe
Influence
numbers of value
the value of
of replacement
aggregate replacement
replacement rate
rate
rate (%).
(%). on WSCC. (a) FA15, (b) FA30. Note-FA is for fly
ash; numbers are the value of replacement rate (%).
Thesurface
The surfaceWSCC
WSCC valuevalue was
was larger
largerthanthanthetheinterior
interior value, which
value, whichstabilized at a at a
stabilized
depth
depth of 30–40
Theofsurface
30–40 mm. mm.
WSCC That
That
valuewas
waswasdue to
duelargera superficial
to a superficial sample
than the interior in
samplevalue,contact
in contactwith the
whichwith solution
the solution
stabilized at a
directly.InInthe
directly. theearly
earlystage,
stage, chloride
chloride ion
ion penetration
penetration ininthe
theconcrete
concrete specimens
specimens waswas
dom-domi-
depth of 30–40 mm. That was due to a superficial sample in contact with the solution
inated by capillary absorption, and the penetration rate was fast [39]. The difference in
nated by
directly. In capillary
the early absorption,
stage, chloride andionthepenetration
penetrationinrate was fast specimens
the concrete [39]. The difference
was domi-in
chloride ion concentration between the internal specimen solution and the immersion
chloride
nated ion concentration between the internal specimen solution
solution narrowed as the specimen became saturated, and chloride ion penetration became in
by capillary absorption, and the penetration rate was fast and
[39]. the
The immersion
difference so-
lution
chloride narrowed
dominated as the specimen
ion concentration
by diffusion, between became saturated,
the internal
with a relatively slow specimen and solution
penetration chloride ion penetration
and
rate. However, thebecause
immersion became
areas so-
dominated
lution narrowed by diffusion,
as the with
specimen a relatively
became slow
saturated,penetration
and rate.
chloride However,
ion
near the erosion surface were always saturated first, the WSCC in the shallow layer of the because
penetration areas
became
near the erosion
dominated
specimen bywas surface
diffusion,
high, were
with
while always saturated
theaconcentration
relatively slow first, thelayer
penetration
in the deeper WSCC wasin
rate. theand
However,
low, shallow layerareas
because
the differenceof the
specimen
nearwas
thenot was high,
significant.
erosion surface while
werethe concentration
always saturatedin the the
first, deeper
WSCC layer wasshallow
in the low, and theof
layer differ-
the
ence waswas
specimen not high,
significant.
while the concentration in the deeper layer was low, and the differ-
3.4.2. WSCC and FA Content
ence was not significant.
Figureand
3.4.2. WSCC 11 shows the effect of fly ash content on WSCC after 3%NS-45FT. It demon-
FA Content
strates
3.4.2. WSCC that WSCC with RBCA dropped dramatically in response to increasing the FA
Figure and FA Content
11 shows the effect of fly ash content on WSCC after 3%NS-45FT. It demon-
dosage and that 30% FA greatly enhanced resistance to chloride-ion penetration compared
strates that
toFigure
15% WSCC
11
FA. shows with
theRBCA
effect dropped
of fly ashdramatically in response
content on WSCC after to increasing the
3%NS-45FT. FA dos-
It demon-
strates that WSCC with RBCA dropped dramatically in response to increasing the FA dos-to
age and that 30% FA greatly enhanced resistance to chloride-ion penetration compared
15%
age andFA.that 30% FA greatly enhanced resistance to chloride-ion penetration compared to
15% FA.
Materials 2021, 14, 7267 0.9 0.9 12 of 16
Materials 2021, 14, 7267 R100-FA0 R80-FA15 12 of 15
0.8 R100-FA15 0.8 R80-FA30
0.7 R100-FA30 0.7
0.6 0.6

WSCC(%)
WSCC(%)
0.5 0.5
0.9 0.9
0.4 R100-FA0
0.4 R80-FA15
0.8 R100-FA15 0.8 R80-FA30
0.3 0.3
0.7 R100-FA30 0.7
0.2 0.2
0.6 0.6
0.1 0.1

WSCC(%)
WSCC(%)
0.5 0.5
0.0 0.0
0 10 20
0.4 30 40 50 0 10 200.4 30 40 50
depth(mm)
0.3 depth(mm)
0.3
0.2 (a) 0.2
(b)
0.1 fly ash content on WSCC. (a) R100, (b) R80. Note—R
Figure 11. Influence of 0.1 is for recycled brick-
0.0
concrete aggregate; numbers are the value of replacement rate (%). 0.0
0 10 20 30 40 50 0 10 20 30 40 50
depth(mm) depth(mm)
3.5. SEM and XRD
(a) (b)
SEM microscopy was used to examine the microstructure of concrete containing
Figure 11. Influence of fly ash content on WSCC. (a) R100, (b) R80. Note—R is for recycled brick-
RBCA. After undergoing
Figure 11. a 3%NS-45FT
Influence treatment
of fly ash content (Figure
on WSCC. 12),
(a)the concrete
R100, (b) R80.specimens be-recycled brick-
Note: R is for
concrete aggregate; numbers are the value of replacement rate (%).
came rather loose, with aggregate;
concrete large holes and noticeable
numbers fissures
are the value visible. rate (%).
of replacement
Differences in microstructure were also detected (see Figure 12a–d), with the concrete
3.5.3.5.
SEM SEMandand
XRDXRD
specimen containing 100% RBCA having larger pores and more cracks. Through repeated
freeze-thaw cycles,SEM SEMmicroscopy
those microscopy was
cracks expanded used
was used andto to examine
examine
interacted the the
thewith microstructure
microstructure
pores of
and of concrete
concrete containingcontaining
interfacial RBCA.
AfterAfter
RBCA. undergoing a 3%NS-45FT
undergoing a treatmenttreatment
3%NS-45FT (Figure 12),(Figure
the concrete
12), specimens
the concretebecame rather be-
specimens
transition zones, providing pathways for ions to permeate the internal structure from the
loose, with large holes and noticeable fissures visible.
came rather loose, with large holes and noticeable fissures visible.
external environment.
Differences in microstructure were also detected (see Figure 12a–d), with the concrete
specimen containing 100% RBCA having larger pores and more cracks. Through repeated
freeze-thaw cycles, those cracks expanded and interacted with the pores and interfacial
transition zones, providing pathways for ions to permeate the internal structure from the
external environment.

(a) (b)

(a) (b)

(c) (d)
Figure 12. SEM image of specimens with RBCA after 3%NS-45FT (1000×). (a) R100-FA15, (b) R100-
Figure 12. SEM image of specimens with RBCA after 3%NS-45FT (1000×). (a) R100-FA15, (b) R100-FA30, (c) R80-FA15,
FA30, (c) R80-FA15, (d) R80-FA30. Note—R is for recycled brick-concrete aggregate; FA is for fly
(d) R80-FA30. Note: R is for recycled brick-concrete aggregate; FA is for fly ash; numbers are the value of
ash; numbers are the value of replacement rate (%).
replacement rate (%).
Differences in microstructure were also detected (see Figure 12a–d), with the concrete
specimen containing(c)100% RBCA having larger pores and more cracks. (d) Through repeated
Figure 12. SEM image of specimens with RBCA after 3%NS-45FT (1000×).pores
freeze-thaw cycles, those cracks expanded and interacted with the and interfacial
(a) R100-FA15, (b) R100-
FA30, (c) R80-FA15, (d) R80-FA30. Note—R is for recycled brick-concrete aggregate; FA is for fly
ash; numbers are the value of replacement rate (%).
 Materials 2021, 14, 7267 13 of 15
Materials 2021, 14, 7267 13 of 16

transition zones, providing pathways for ions to permeate the internal structure from the
external
Afterenvironment.
45 freeze-thaw cycles, concrete specimens containing 80% RBCA had a denser
matrix than45
After freeze-thaw
those cycles,
containing concrete
100%, specimens containing
but specimens containing 80%15%RBCA
FA were had inferior
a denserto
matrix than those containing 100%, but specimens containing 15% FA
those containing 30% FA. This suggested that concrete with 15% FA was more susceptiblewere inferior to those
containing 30% FA. This suggested that concrete with 15% FA was more
to chloride attack, whereas concrete with 30% FA exhibited stronger chloride ion penetra- susceptible to
chloride
tion attack,Generally,
resistance. whereas concrete with 30%
microscopic FA exhibitedmatched
characteristics strongermacroscopic
chloride ion penetration
examination
resistance. Generally,
results (WSCC test). microscopic characteristics matched macroscopic examination results
(WSCC test).
X-ray Diffraction (XRD) patterns were used to determine the phase composition of
X-ray Diffraction (XRD) patterns were used to determine the phase composition of
concrete containing RBCA that was subjected to sodium chloride solutions during freez-
concrete containing RBCA that was subjected to sodium chloride solutions during freezing-
ing-thawing cycles. As presented in Figure 13, the samples all had similar diffraction
thawing cycles. As presented in Figure 13, the samples all had similar diffraction peaks
peaks in terms
in terms of typeof and
typeposition,
and position, indicating
indicating no new nophases
new phases
formedformed in the
in any of anyspecimens.
of the spec-
imens. The distinctive
The distinctive peak ofpeak
SiO2 ,oforiginating
SiO2, originating
from sand,fromwassand, was the
the most most prominent,
prominent, followed by fol-
lowed by Ca(OH) 2, AFt (3CaO·Al 2O3 CaSO 4·32H2O), and
Ca(OH)2 , AFt (3CaO·Al2 O3 CaSO4 ·32H2 O), and Friedel’s salt (3CaO·Al2 O3 ·CaCl2 ·10H2 O, Friedel’s salt
(3CaO·Al 2O3·CaCl
abbreviated 2·10H
as Fs). 2O,
The abbreviated
presence as Fs). salt
of Friedel’s Theinpresence
the XRDofgraph
Friedel’s salt inthat
suggested the the
XRD
graph suggested that the chloride salt had penetrated the matrix and
chloride salt had penetrated the matrix and reacted with the AFm phase [40,41]. Moreover, reacted with the
AFm phase [40,41].
FA reacted with theMoreover,
Ca(OH)2 phaseFA reacted
to formwith
C-S-H,thea Ca(OH) phase
reaction 2that to form
appeared to C-S-H, a reac-
be related to
tion
thethat appeared
chloride to be related
ion’s physical to the chloride
adsorption capacity ion’s physical adsorption capacity [42–44].
[42–44].

--Fs --AFt --SiO2 --Ca(OH)2

R100-FA15
Intensity/(a.u.)

R100-FA30

R80-FA15

R80-FA30
     
    

20 25 30 35 40 45 50 55
2/degree(°)
Figure
Figure13.
13.XRD
XRDpatterns
patternsof
ofspecimens
specimens exposed 3%NS-45FT.
exposed to 3%NS-45FT.

4.4.Conclusions
Conclusions
Concrete containing RBCA and FA were evaluated comprehensively after being
Concrete containing RBCA and FA were evaluated comprehensively after being sub-
subjected to a combined 3% sodium chloride solution and 45 freeze-thaw cycle regime
jected to a combined 3% sodium chloride solution and 45 freeze-thaw cycle regime
(3%NS-45FT). Based on the compressive strength, mass loss rate (MLR), relative dynamic
(3%NS-45FT). Based on the compressive strength, mass loss rate (MLR), relative dynamic
elastic modulus (RDEM), water-soluble chloride content (WSCC), SEM, and XRD, the
elastic modulus
following (RDEM),
conclusions canwater-soluble
be made: chloride content (WSCC), SEM, and XRD, the fol-
lowing conclusions can be made:
1. The replacement of virgin aggregates with RBCA composed of 30% recycled brick ag-
1. The replacement
gregate and 70% of virginconcrete
recycled aggregates with RBCA
aggregate led to acomposed
decrease inof
28 30%
daysrecycled brick
compressive
aggregate
strength.and
The70%
R80 recycled concrete
series concrete aggregate
had a marginled to a decrease
of increase in 28 days
of 2.2–7.9% thancompres-
that of
sive strength.
R100 The R80 The
series concrete. series concrete
best dosage had
of FAa in
margin of increase
combination withof 2.2–7.9%
recycled than that
aggregate
ofwas
R100 series concrete.
discovered The best dosage of FA in combination with recycled aggre-
to be 15%;
2. gate wasthe
When discovered to be 15%;
RBCA content increased from 80% to 100%, concrete specimens were
2. When susceptible
the RBCAto more damage
content basedfrom
increased on the increased
80% to 100%, MLR and sharper
concrete reduction
specimens in
were sus-
RDEM.to
ceptible The concrete
more damageMLRbased
was lowest
on thewith 15% FA,MLR
increased whileand
RDEM loss was
sharper lowestin
reduction
with 30%
RDEM. TheFA. The addition
concrete MLR was of 15% FA improved
lowest with 15%the FA,resistance of concrete
while RDEM loss following
was lowest
with 30% FA. The addition of 15% FA improved the resistance of concrete following
3% NS-45FT, while the RDMA of various RBCA concrete varied according to the
amount of FA;
Materials 2021, 14, 7267 14 of 15

3% NS-45FT, while the RDMA of various RBCA concrete varied according to the
amount of FA;
3. All WSCC followed the same trend, decreasing within 30 mm of the sodium chloride-
eroded surface, recovering slightly, and reaching a constant value in the area beyond
30 mm. The chloride penetration resistance of concrete containing 30% FA was the
best, owing to the concrete’s low WSCC value.

Author Contributions: Conceptualization, D.W.; methodology, D.W.; software, N.W. and Y.Y.; vali-
dation, Z.M., C.W. and X.Z.; formal analysis, D.W. and Y.Y.; investigation, J.W. and Y.Y.; resources,
J.W.; data curation, J.W.; writing—original draft preparation, Y.Y.; writing—review and editing, D.W.
and Y.Y.; visualization, J.W.; supervision, D.W.; project administration, D.W.; funding acquisition,
D.W. All authors have read and agreed to the published version of the manuscript.
Funding: The authors would like to acknowledge the National Natural Science Foundation of China
(through the grant 51968060); Key Research and Development Plan of Ningxia (2018BFH03003); First
Class Discipline Project of Ningxia Higher Education Institution (NXYLXK2021A03); and Natural
Science Foundation of Ningxia (2020A1142).
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: The data presented in this study are available on request from the
corresponding author.
Conflicts of Interest: The authors declare no conflict of interest.

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