Journal of Building Engineering 90 (2024) 109473

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Journal of Building Engineering

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

Carbonation curing behavior and performance improvement of

recycled coral waste concrete
Yi-Sheng Wang a, Shafiq Ishak b, Guang-Zhu Zhang c, **, Xiao-Yong Wang a, d, *
a
Department of Integrated Energy and Infra System, Kangwon National University, Chuncheon-si, 24341, Republic of Korea
b
Department of Structure and Materials, Faculty of Civil Engineering, University of Technology Malaysia (UTM), Johor Bahru, 81310, Johor,
Malaysia
c
School of Civil Engineering and Transportation, Northeast Forestry University, Harbin, 150040, China
d
Department of Architectural Engineering, Kangwon National University, Chuncheon-si, 24341, Republic of Korea

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

Keywords: Carbonation curing can improve material properties and reduce the concrete industry’s carbon
Carbonation curing emissions. This study used powder prepared from waste coral to replace ordinary Portland cement
Coral powder (0, 10, and 20 %). After initial curing for 24 h, the mortar was cured by sealing and carbonation.
Dilution effect The dilution effect of coral powder substantially reduces the mechanical properties under sealing
Sustainability curing. Under carbonation curing, the coral powder helps develop carbonation and CO2 diffusion,
Durability
reducing strength loss and increasing resistivity. XRD and Fourier transform infrared spectroscopy
analysis results showed that carbonation transforms hydration products and clinker phases into
different types of CaCO3, such as calcite and aragonite. The novelty of this study is that it proposes
a method that organically combines carbonation curing and marine waste reuse. Provide a sus­
tainable solution to the problem of material shortage in marine engineering construction.
Moreover, the carbon footprint can be considerably reduced by replacing cement materials,
improving carbonation curing efficiency, and promoting CO2 uptake.

1. Introduction
Carbonation curing of concrete is currently a vital carbon sequestration technology in the construction field [1–4]. This technology
refers to curing cement-based materials by exposing them to an environment rich in CO2 and a specific relative humidity (50–70 %).
The carbonation reaction mainly includes two processes: diffusion and reaction of CO2 [5]. When the internal relative humidity of the
cement-based material is higher than 70 %, most of the capillaries are in a saturated state; the diffusion rate of CO2 is slow, and it
controls the carbonation reaction. When the relative humidity is lower than 50 %, the water content of most capillaries is insufficient;
the CO2 reaction speed is slow, and the chemical reaction of CO2 controls the carbonation reaction. Generally, when the relative
humidity is in the range of 50%–70 %, the speed of CO2 diffusion and CO2 reaction is relatively fast; macroscopically, the carbonation
reaction is the fastest.
In addition to the influence of relative humidity mentioned above, the effect and rate of carbonation curing are strongly affected by
various factors, including CO2 concentration, curing time, curing temperature, and concrete mix ratio. The study by Shi et al. showed
that appropriate CO2 concentration and curing time can significantly improve the strength of concrete [6]. High temperature and high

* Corresponding author.
** Corresponding author.
E-mail addresses: [email protected] (G.-Z. Zhang), [email protected] (X.-Y. Wang).

https://doi.org/10.1016/j.jobe.2024.109473
Received 26 February 2024; Received in revised form 19 April 2024; Accepted 27 April 2024
Available online 29 April 2024
2352-7102/© 2024 Elsevier Ltd. All rights reserved.
Y.-S. Wang et al. Journal of Building Engineering 90 (2024) 109473

pressure environments may accelerate the carbonation reaction rate [7]. As a more environmentally friendly concrete curing method,
carbonation curing stores CO2 in the building material for a long time. With in-depth research on its impact mechanism and process,
carbonation curing will provide more efficient and reliable construction solutions for concrete projects. The carbonation reaction can
be summarized as gaseous CO2 dissolution and ionization to produce carbonate ions; hydration products dissolve in capillary water to
produce calcium ions, followed by dissolution of unhydrated clinker. Carbonate ions and calcium ions react to produce CaCO3.
Equations (1)–(5) detail the carbonation reaction of hydrated products and unhydrated clinker [8]. As a more environmentally friendly
concrete curing method, carbonation curing stores CO2 in the building material for a long time. With in-depth research on its impact
mechanism and process, carbonation curing will provide more efficient and reliable construction solutions for concrete projects.

Ca(OH)2 + CO2 → CaCO3 + H2O (1)

3CaO⋅Al2O3⋅3CaSO4⋅32H2O + 3CO2 → Al2O3⋅xH2O + 3CaCO3 + 3(CaSO4⋅2H2O) + (26-x)H2O (2)

3CaO⋅2SiO2⋅3H2O + 3CO2 → 3CaCO3 + 2SiO2⋅3H2O (3)

3(3CaO⋅SiO2) + 3CO2 + nH2O → 3CaCO3 + SiO2•nH2O (4)

2(2CaO⋅SiO2) +2CO2 + nH2O → 2CaCO3 + SiO2•nH2O (5)

In recent years, researchers have become increasingly interested in other calcareous material. Calcareous materials mainly refer to
compounds with high calcium content and have the potential to be used as cement replacement materials. Limestone is a common
carbonate sedimentary rock that has been used in cement-based materials for many years. The addition of finely ground limestone to
cement has been recognized by many standards, such as ASTM C150 [9], European Standard EN 197–1 [10], and the Canadian
Standards Association (CSA) [11]. Ground granulated blast-furnace slag (GGBFS) is a by-product of the blast-furnace pig iron
manufacturing process; fly ash is a solid waste from coal-fired power plants. They are also commonly used calcium materials in cement.
Because of its pozzolanic activity, GGBFS can react with calcium hydroxide to form a cementitious material that improves the strength
and durability of concrete [12]. According to the different calcium content, Fly ash can be divided into high calcium fly ash (CaO
exceeds 15–20 %, class C) and low calcium fly ash (CaO less than 10 %, class F) [13]. Fly ash is slightly less reactive but can improve the
slump of concrete [14]. In addition, some wastes with high calcium content can also be used to replace cement after processing, such as
coral, eggshells, and shells [15–17]. As early as the 20th century, coral aggregate concrete was applied in the United States [18].
Recent studies have shown that using coral powder (CP) to replace cement partially reduces the total manufacturing cost and carbon
emissions. Shi et al. studied the effect of CP on the hydration of Portland cement and noted that it has similar hydration properties and
effects as limestone [19].
With the development of marine engineering, an increasing demand for building materials in projects such as reclamation, island
building, and dock construction [20]. Since the island lacks concrete raw materials, it needs to be transported inland; this adds a lot of
labor and time costs, as well as carbon emissions from transportation [21]. Using local materials can solve the shortage of raw ma­
terials; the large amount of coral waste generated during marine engineering has become a potential reuse resource. The chemical
composition of coral is mainly aragonite and calcite, with a CaCO3 content of 98 % [22]. Coral waste and limestone have similar
chemical compositions. However, limestone mainly comes from inland mining. Limestone is difficult to use widely in marine con­
struction projects, considering the transportation cost. Therefore, using CP as an alternative material to cement in marine engineering
has become a more viable option. This strategy helps solve the problem of shortage of raw materials in marine engineering and reduces
pollution of the marine environment [23,24].
However, it should be pointed out that adding CP as a low-reactivity filler will reduce cementitious materials and produce a dilution
effect [25]. It has been reported that addition levels exceeding 5 % reduce the mechanical properties of mortar [19]. In addition,
adding a large amount of CP increases the porosity of concrete or mortar, which is not conducive to durability development [26,27].
These limitations make the widespread application of CPs in island construction challenging. Methods for improving the properties of
OPC-CP cement-based materials are needed to maximize the potential of coral waste. As confirmed by previous studies [8,28],
carbonation curing is an effective method for improving density and strength of a material. However, to the best of the authors’
knowledge, systematic studies on the carbonation curing behavior and microscopic and property development of OPC-CP mixtures are
lacking. Related research is needed to determine the actual effect of this approach.
In summary, based on the limitations of the application of CP in marine engineering and the shortcomings of current research, this
study proposes a method for using carbonation curing technology to improve the performance of OPC-CP mortar. The investigation
compared the performance of mortar prepared by two curing methods, sealing and carbonation, with different CP substitution levels
(0, 10, and 20 %). Isothermal calorimetry was used to monitor slurry hydration. The carbonation degrees were measured, and the CO2
uptake was calculated to assess sustainability. Thermogravimetric (TG), X-ray diffraction (XRD), and Fourier transform infrared (FT-
IR) spectroscopy analyses were used to characterize the mineralogy. The microstructural morphology was observed by scanning
electron microscopy (SEM). The macroscopic properties, such as strength, ultrasonic pulse velocity (UPV), and resistivity, were sys­
tematically tested. The method proposed in this study can enhance the mechanical properties and durability of OPC-CP mortar. In
addition, this study provides a more attractive strategy for applying CPs in the marine engineering. Moreover, the environmental
benefits of building materials are doubled by replacing cement, improving carbonation efficiency, and promoting multiple mecha­
nisms of CO2 uptake.

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Y.-S. Wang et al. Journal of Building Engineering 90 (2024) 109473

2. Experimental study
2.1. Raw materials
The raw waste coral used in this study was obtained from Jeju Island, South Korea, and ground into coral powder by a ball mill in
the laboratory. The waste coral was ultrasonically cleaned for 48 h before grinding to remove residual sludge on the surface. Crush the
waste coral into particles, put it into a ball mill, and grind it at 500 rpm for 15 min. The resulting powder was then passed through a 45-
μm sieve to obtain CP that could be used for experiments. The production process of the CP, XRD, and microscopic morphology are
shown in Fig. 1.
Untreated waste coral has a porous structure on a macroscopic scale. After grinding and sieving, the D50 particle size of CP reaches
micron level size (6.54 μm, Fig. 2). The micromorphology of CP after magnification of 20,000 times is shown in the SEM in Fig. 1 (c):
grinding eliminates the porous structure of coral; finely ground coral powder has no porous and can be used as replacement materials
for OPC. In addition, XRD analysis results show that the composition of CP is CaCO3, mainly composed of aragonite mixed with a small
amount of calcite. It is reported that although it is also CaCO3, limestone is primarily composed of calcite, which is the main difference
between CP and limestone.
The Type I cement (OPC) used in this study was purchased from Sung Shin Cement Company in South Korea. The particle size
distribution of the raw material detected using a particle size tester is shown in Fig. 2. The chemical compositions of the CP and OPC
samples determined using an X-ray fluorescence spectrometer are shown in Table 1. Table 2 shows the aggregate properties of standard
sand.

2.2. Mixture preparation

CP replaced OPC at 0, 10, and 20 % of the cement mass. The mixture was prepared using a water–binder ratio of 0.5. The mixtures
used for macroscopic analysis (mechanical properties, UPV, and resistivity) were made of mortar with a sand–binder ratio of 2.75. The
pastes were subjected to microscopic analysis (hydration heat, SEM, TG, XRD, and FT-IR). Microscopic samples used for carbonation
curing are made into paste sheets about 1 mm thick and placed in a carbonation curing box. Because the prepared sample is thin, it is
guaranteed to be carbonated entirely after 28 d. The detailed mix proportions and curing methods are shown in Table 3. The numbers
in the sample names represent the substitution level of CP. S and C represent the curing methods used for the sample.
The preparation process of the mixture was as follows: First, the weighed materials were put into the mixer in sequence and mixed
for 60 s to ensure that the raw materials were evenly mixed. After pouring the weighed mixing water into the mixer, the mixture was
mixed at a stirring speed of 60 rpm for 120 s. The remaining mixture on the inner wall and bottom of the mixer was scraped off, and
mixing was continued for 120 s using a stirring speed of 120 rpm. The obtained uniform mixture was poured into the prepared molds
(5 × 5 × 5 cm and 4 × 4 × 16 cm) and vibrated gently to eliminate air bubbles. The mixture was covered with a film and placed in an
indoor environment at 20 ± 1 ◦ C for curing.

Fig. 1. Production process (a), XRD (b), magnifies 20000 (c), and 5000 times microscopic morphology (c) of the coral powder.

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Fig. 2. Particle size distribution of the cement and coral powder.

Table 1
Chemical composition of the cement and coral powder.

Chemical composition (mass%) Cement Coral powder

CaO 63.1 53.68

MgO 2.31 0.31
Al2O3 4.96 0.25
SiO2 21.0 0.75
P2O5 0.116 0.02
SO3 2.31 0.57
K2 O 0.910 0.03
Cl – 0.03
TiO2 0.278 –
MnO 0.0877 0.6
Fe2O3 2.77 0.13
ZnO 0.0646 –
Loss on ignition 2.06 43.62

Table 2
Aggregate properties of the Standard sand.

Properties Values

Specific gravity 2.62

Moisture content 0.18 %
Water absorption 0.59 %
Bulk Density 1628 kg/m3

Table 3
Mix proportions of the cement blends.

Cement Coral powder W/B S/B Curing method

CP0–S 100 0 0.5 2.75 Sealing

CP10–S 90 10 0.5 2.75 Sealing
CP20–S 80 20 0.5 2.75 Sealing
CP0–C 100 0 0.5 2.75 Carbonation
CP10–C 90 10 0.5 2.75 Carbonation
CP20–C 80 20 0.5 2.75 Carbonation

2.3. Curing method

The entire curing process in this study was divided into two stages, namely, before sample demolding (first 24 h) and after
demolding (24 h—test age). All the samples were cured in molds at 20 ± 1 ◦ C for 24 h. To study the interaction between curing
methods and CP content, the methods after demolding were divided into two types: (1) The samples were sealed with polyethylene
film, transferred to a standard curing box at 20 ◦ C for sealing curing. (2) The samples were transferred to a carbonation curing box for

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Y.-S. Wang et al. Journal of Building Engineering 90 (2024) 109473

carbonation curing. The specific curing process, sample type, and test methods are shown in Fig. 3.
The curing conditions selected in this study are 10 % CO2 concentration and 20 ◦ C; according to Seo et al. [29], this curing
condition is beneficial to the carbonation of cement-based materials. The samples were placed in a carbonation curing box equipped
with a temperature and CO2 concentration adjustment device to maintain a constant CO2 concentration of 10 % and 20 ± 1 ◦ C.
Carbonation curing releases considerable moisture, which can affect the penetration process and reactions. Therefore, super absorbent
polymers are placed at the bottom of the carbonation box to absorb the water generated during the carbonation curing process. In
addition, a saturated sodium bromide solution was prepared to maintain the relative humidity in the carbonation curing box at 60 ±
2.5 %; a humidity sensor was installed in the curing box to monitor changes in relative humidity.
It should be pointed out that there are many methods of carbonation curing. Previous studies investigated the curing method using
99.9 % CO2 in 1 atm for 2, 4, and 96 h and at 4 atm for 24 h [30,31]. Although the methods used in these studies have short curing
times, the experimental operation is relatively complicated [32,33]. First, the sample needs to be pretreated before carbonation curing.
Second, if the curing time is too short, the carbonation effect will not be noticeable; if the curing time is too long, drying shrinkage may
easily occur. Finally, post-treatment is required after carbonation curing, usually water replenishment. However, until now, there has
been no clear regulation or consensus on post-processing. The 28 d 10 % CO2 concentration curing method may be uneconomical;
however, this method has the following advantages: 1. It facilitates the demoulding of concrete products; 2. It omits the pre-curing
treatment before carbonation curing and the subsequent water replenishment process; 3. Only a 10 % concentration of CO2 is
required, which can save the cost of CO2 high-pressure liquefaction and purification. It can even be cured directly with industrial flue
gas, which is conducive to promotion in actual projects. After comprehensively comparing the advantages and disadvantages of
different curing methods, the 28 d 10 % CO2 concentration curing method was adopted in this study [29].

2.4. Experimental methods

2.4.1. Isothermal calorimetry
A multichannel isothermal calorimeter was used to monitor the heat release of the slurry to study the effect of CP on the hydration
kinetics of the OPC. The cement slurry was mixed at 20 ◦ C, and approximately 5 g was sealed in ampoules and placed in different
calorimeter channels. The test was conducted under isothermal conditions at 20 ± 0.02 ◦ C and lasted 168 h.

2.4.2. Carbonation degree and CO2 uptake calculation

The pH of concrete materials is usually approximately 12.5, and carbonation reactions cause the pH of concrete to drop below 9.
Phenolphthalein reagent is colorless when the pH of the test subject is less than 9 and appears magenta when the pH is above 10.5. This
property makes phenolphthalein ideal for distinguishing between carbonated and noncarbonated regions [4]. At different carbonation
curing ages, a 4 × 4 × 16 cm sample was cut off, and phenolphthalein reagent was sprayed on the cross section. The carbonation degree
(%) was calculated based on the ratio of the carbonated area to the noncarbonated area.
In addition, CO2 uptake (%) is defined as the ratio of the mass of CO2 sequestered during carbonation per g of cement. The amount
of carbonation product (CaCO3) can be calculated based on the TG results. The CO2 uptake of carbonated samples can thus be
calculated from the stoichiometric composition of CaCO3.

2.4.3. Phase identification

Carbonation-cured and seal-cured samples were crushed and ground to a particle size of less than 63 μm. Then, the samples were
immersed in isopropyl alcohol solution to stop the reaction. The processed samples were filtered and placed in a vacuum box to dry in
preparation for phase identification. Thermogravimetric analysis of the dried powder was performed using a TG analyzer. Approxi­
mately 20 mg of powder was used per run. Tests were performed under nitrogen purge over a 50–1050 ◦ C range and a heating rate of

Fig. 3. Curing process, sample types and test methods.

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10 ◦ C/min. Mineralogical analysis of the powder was performed using an X-ray diffractometer. The intensity of the diffraction peaks of
the crystals contained in the material was determined by scanning in the range of 5–45◦ 2θ at a scan rate of 0.05◦ 2θ/s. An FT-IR
spectrometer was used to scan the bands corresponding to functional groups in the powder at 500-1900 cm− 1. Each sample was
scanned 64 times.

2.4.4. Micromorphological observation

The micromorphology of the carbonation-cured and sealed-cured samples was observed using a scanning electron microscope. An
FESEM TESCAN MIRA microscope was used for the study. Before starting the test, the sample needs to be platinum coated to improve
its imaging performance during SEM.

2.4.5. Mechanical properties and durability

Three 5 × 5 × 5 cm mortars were used for compressive strength testing according to standard ASTM C109 on days 3, 7, and 28 of
curing (including the 24 h in-molds curing). An AGX-600 universal material testing machine was used in the experiment. The
compressive strength was calculated as the average of the three tests.
The UPV can be used as an aid in assessing the strength development of mixtures. Testing was conducted following AASHTO T 358.
The sample was placed between the ultrasonic transmitter and receiver, and the coupling agent was evenly applied to ensure a
complete surface fit.
Carbonation curing has both positive and negative effects on the corrosion of steel bars related to chloride ion intrusion in concrete
[34]. On the one hand, the products after carbonation curing of cement are CaCO3 and amorphous silica. Compared with hydration
products, the carbonation products have lower chloride ion binding ability and are prone to increased corrosion of steel bars. On the
other hand, carbonation curing can refine concrete pores and reduce the chloride ion diffusion coefficient, thereby increasing corrosion
resistance. Therefore, the overall impact of carbonation curing on steel corrosion by chloride ion intrusion needs to be further
determined. The surface resistivity can be used to assess the corrosion resistance of building materials. Test surface resistivity was
tested according to RILEM TC154-EMC using a four-point probe tester. The dimensions of the tested sample were 4 × 4 × 16 cm, and
the sample surface was cleaned before testing.

3. Experimental results analysis

3.1. Hydration kinetics
The effect of CP on the hydration kinetics of OPC within 168 h is shown in Fig. 4. The initial dissolution peak (peak 1) was observed
for all the samples. The main peak (peak 2) appears at approximately 9 h, and the shoulder peak (peak 3) follows. The main peak
corresponds to the hydration of C3S and the growth of CSH, and the shoulder peak corresponds to the redissolution of C3A and the
precipitation of ettringite [35]. An increase in CP substitution decreases the heat flow of the main and shoulder peaks. This decrease is
attributed to the reduced OPC dosage and the dilution effect produced by CP [36]. Therefore, the increasing substitution level also
causes the cumulative heat to decrease sequentially, as shown in Fig. 4 (b). When CP increases from 0 to 10 % and 20 %, the binder’s
168 h cumulative heat decreases from 315.34 J/g to 297.91 J/g and 278.28 J/g.
The heat flow was normalized to the heat released per g of cement according to Equation (6).
hydration heat
Normalized heat = , (6)
(1 − PCP )

where hydration heat represents the hydration heat flow or cumulative heat measured during the experiment. PCP represents the
substitution level of CP. The normalized results can provide a clearer understanding of the impact of the CP substitution level on
cement hydration.
As the normalization results show (Fig. 5), CP replacement accelerates and enhances the heat flow at the main and shoulder peaks.

Fig. 4. Hydration heat of the OPC-CP mixture.

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Fig. 5. Normalized hydration heat of the OPC-CP mixture.

Moreover, an increase in cumulative heat can be observed. The 168 h normalized cumulative heats of CP0, CP10, and CP20 are 315.34,
331.01, and 347.86 J/g cement, respectively. These observations reveal that CP can function as a nucleation site for CSH [37]. This
ability is mainly attributed to the smaller particle size of CP, which provides an additional specific surface area for the precipitation of
hydration products [38].

3.2. Carbonation efficiency assessment

3.2.1. Carbonation degree
The carbonation degree of the sample can be visually and quickly compared by observing the size of the uncolored area (carbonated
zone) after spraying phenolphthalein. The carbonation degree is calculated based on the ratio of the carbonation zone area to the cross-
sectional area. The calculation method is shown in Equation (7). The phenolphthalein spray test and the corresponding carbonation
degrees at 3, 7, and 28 d curing ages are shown in Fig. 6.

Fig. 6. Evolution of the phenolphthalein color test and carbonation degree.

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carbonation zone area

Carbonation degree = , (7)
cross − sectional area
Carbonation curing of concrete is a process in which CO2 gradually diffuses from the surface into the interior and reacts with the
material. The evolution of the carbonation degree illustrates this point well. At 3 d, the region near the edge of the cross section is first
carbonated and becomes colorless. The center is magenta, indicating that it has not yet been significantly affected by carbonation. At 7
d, as CO2 diffuses from the surface to the center, the carbonation area further increases. The color development area is smaller for the
samples doped with CP, and the carbonation degree is correspondingly greater. This result is attributed to the following: (1) Partially
replacing OPC with CP increases the effective water–cement ratio (w/c) (dilution effect), and the spacing between cement clinkers
increases with the effective w/c [36]. This behavior increases the porosity and diffusion coefficient, facilitating the diffusion of CO2
into the mixture. (2) Studies have shown that CaCO3 (the main component of CP) can serve as a nucleation site for carbonation
products, facilitating precipitation [39,40].
At 28 d, the central area of CP0–C was magenta (uncarbonated zone), the color-developing area of CP10–C was tiny, and CP20–C
appeared colorless. The carbonation degree of the sample without CP incorporation reached 87.9 % at 28 d. When the CP substitution
level was 10 %, the mortar was almost completely carbonated after 28 d, for a carbonation degree of 98.4 %. When the substitution
level was increased to 20 %, the mortar was completely carbonated (carbonation degree 100 %) after curing for 28 d. It is reasonable to
speculate that the time needed for complete carbonation of CP20–C could be substantially reduced (much less than 28 d). These
observations indicate that CP plays a key role in promoting the carbonation process and helps improve the carbonation curing effi­
ciency of mortar.

3.2.2. TG analysis and CO2 uptake calculation

The TG curve can be obtained by testing the relationship between the mixture weight and the temperature, and the DTG curve can
be obtained through its first derivative. The TG and DTG curves of the sealed and carbonated samples are shown in Fig. 7.
As shown in Fig. 7 (a), the DTG analysis of the sealing cured samples revealed three obvious mass losses. The first one is located
within 50–200 ◦ C and is attributed to the dehydration of AFt, AFm, and CSH [41]. The weight loss within 400–450 ◦ C is related to the
dehydroxylation of CH. The third weight loss is related to the decomposition of CaCO3 between 500 and 800 ◦ C [42]. This weight loss
becomes more obvious with increasing CP content because CaCO3 is the main component of CP.
The carbonation reaction causes the decalcification of CSH to produce silica gel, CaCO3, and water. After carbonation, AFt and AFm
generate various compounds, such as CaCO3, gypsum, alumina gel, and water. CH combines with CO2 to generate CaCO3 and water.
Therefore, as shown in Fig. 7 (b), the weight loss at 50–200 ◦ C under carbonation curing conditions is lower than that at other
temperatures, and the weight loss of CH is challenging to observe. In addition, since CaCO3 is the main product of carbonation curing,

Fig. 7. TG and DTG curves of the (a) sealed and (b) carbonated samples.

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its decomposition peak is more obvious than that of sealing curing. The decomposition peak shifts to a higher temperature range
because the CaCO3 produced after vigorous carbonation curing has good crystallinity [43]. A wider decomposition range indicates that
different forms of CaCO3, such as amorphous CaCO3, aragonite, and calcite, may be present [44].
According to the methods proposed in previous studies [45], the TG results can be used to calculate the bound water (BW) and
CaCO3 content (wt. %) in the sample, as shown in Equations (8) and (9).
w50 − w500
Bound water = , (8)
w500

w500 − w800 100

Calcium carbonate = × (9)
w500 44

where w50, w500, and w800 represent the weight of the sample heated to 50, 500, and 800 ◦ C, respectively. The factor of 100
44 represents
the molar mass ratio of CaCO3 to CO2.
In addition, the CO2 that can be stored per g of cement in the carbonated sample is the CO2 uptake. This property can be calculated
from the stoichiometry of CaCO3 produced by the reaction, as shown in Equation (10) [46].
(CCĈ − SCĈ ) 44
CO2 uptake = × , (10)
(1 − PCP ) × mass 100

where CCĈ and SCĈ represent the CaCO3 content in the samples under carbonation and sealing curing, respectively. PCP represents the
44
substitution level of CP. The mass represents the weight of the initial sample. The factor of 100 represents the molar mass ratio of CO2 to
CaCO3.
The BW content in the sealed and carbonated samples was calculated by Equation (8), and the CO2 uptake was calculated according
to Equation (10); the results are summarized in Table 4. The BW content in the sealed sample decreased slightly as CP increased,
consistent with the phenomenon reflected by the decreases in hydration heat flow and cumulative heat. Owing to the low reactivity of
CP, adding 10 and 20 % CP to the cementitious material increased the effective w/c from 0.5 to 0.56 and 0.63, respectively. Moreover,
the corresponding hydration products decreased as the clinker dosage decreased, decreasing the BW content. The BW content was
substantially lower under carbonation curing than under sealing curing. As shown in Equations (1)–(3), this result can be explained by
the carbonation reaction consuming the hydration products.
As CP increases, CO2 uptake increases from 27.32 % to 33.76 % and 36.97 %. The following three points can explain the more
significant CO2 uptake effect: (1) A higher effective w/c increases the spacing between clinker particles, thereby increasing the pores
and diffusion coefficient [26], which benefits the internal diffusion of CO2. (2) A higher porosity means more space is available for the
precipitation of carbonation products. (3) The main component of CP is CaCO3, which can reduce the interfacial energy of carbonation
product precipitation and play a nucleation role [39]. This behavior induces more carbonate precipitation, which is beneficial for CO2
uptake.

3.3. Mechanical properties

Fig. 8 shows the strength development of the samples under two curing methods (a, b). To clarify the promoting effect of the
carbonation curing method on strength increase, the relative strength results (c, d) based on the strength of the control sample (CP0–C/
S) are given. The relative strength is calculated according to Equation (11).
SCPX
S relative = × 100, (11)
SCP0

where S relative represents the relative strength and SCPX and SCP0 represent the strengths of the samples with different CP contents and
without CP, respectively.
Under sealing curing conditions, the compressive strength decreased with increasing substitution level of CP. This decrease in
strength is attributed to the following two points: (1) The main component of CP is CaCO3, which has low reactivity [47]. Therefore,
the dilution effect of adding CP increases the effective w/c. The strength of concrete is often inversely related to the w/c since more
water means higher porosity [19]. (2) Since the addition of CP reduces the amount of clinker, the amount of hydration products per
unit volume decreases accordingly. The decrease in BW content calculated by TG was sufficient to confirm this inference. Although the

Table 4
Effective w/b, BW (wt. %), and CO2 uptake (wt. %).

Curing method Sample Effective w/c BW CO2 uptake

Sealing CP0–S 0.5 24.03 –

CP10–S 0.56 22.42 –
CP20–S 0.63 21.21 –

Carbonation CP0–C 0.5 11.03 27.32

CP10–C 0.56 9.49 33.76
CP20–C 0.63 9.2 36.97

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Fig. 8. Strength of mortars under sealing and carbonation curing conditions.

CP accelerates and improves hydration (based on the normalized hydration heat result). However, at dosages of 10 and 20 %, the
increase in strength resulting from the filler effect cannot offset the negative impact of the dilution effect on strength.
As shown in Fig. 8 (a, b), carbonation curing is very effective at improving the strength of concrete. In addition, the normalized
results show that the carbonated sample has a higher normalized strength than the sealed sample (Fig. 8 (c, d)). At 28 d, the relative
strengths of CP10 and CP20 under sealing and carbonation curing were 75.3 % and 56.2 % and 84.2 % and 67.1 %, respectively.
Compared with those of sealing curing, the 28-d relative strengths of CP10 and CP20 increased by 8.9 % and 10.9 %, respectively,

Fig. 9. XRD of sealed and carbonated samples.

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under carbonation curing. In other words, carbonation curing can partially compensate for the negative impact of dilution on strength.
According to the carbonation degree test, CP reduces the difficulty of CO2 diffusion through the dilution effect. Moreover, by
reducing the interfacial energy of carbonation product precipitation, more CaCO3 precipitation occurs [39,48]. The molar volume of
carbonation products is larger than that of hydration products, where the transformation of CH to CaCO3 will result in a volume
increase of approximately 11.8 % [49]. These carbonation products may precipitate on the surface of the calcium-rich phase or in the
micropores of the matrix, increasing the compressive strength. These observations illustrate that carbonation curing improves the
mechanical properties of OPC-CP mixtures and effectively improves their safety.

3.4. Phase identification

3.4.1. XRD
The XRD patterns obtained under the two curing methods are shown in Fig. 9. Typical hydration products can be observed in seal-
cured samples. For example, AFt (2 θ = 9.2) is generated from aluminate hydration, and CH (2 θ = 18.1, 34.2) is generated from silicate
hydration. MC (2 θ = 11.7) is produced by the hydration of aluminates and CaCO3 contained in OPC. Since the OPC used contains a
small amount of calcite, weaker diffraction peaks (2 θ = 23.1, 29.5) are detected in the CP0–S sample. In addition to calcite, aragonite
(2 θ = 26.3) from the CP was also detected in the CP10–S and CP20–S samples. In addition, some unhydrated clinker phases, namely,
C3S and C2S (2 θ = 32.2, 32.6, 41.2), still existed in the 28-day sealed sample.
These observations indicate that the carbonation curing of cement-based materials is essentially a CO2 sequestration process. The
hydration products and clinker are consumed after carbonation, and a large amount of CaCO3 is formed, as described in Equations (1)–
(5). Through comparison, it is seen that the diffraction peaks of AFt and Mc disappear under carbonation curing conditions. The in­
tensity of the diffraction peaks corresponding to C3S, C2S, and CH decreased considerably. Moreover, the diffraction peak density of
CaCO3 (calcite and aragonite) increases considerably, and CaCO3 becomes the most important crystalline phase. After carbonation
curing, aragonite was also detected in sample without CP incorporation due to carbonation of the hydration products and clinker. The
common increase in calcite and aragonite diffraction peaks confirmed that the CaCO3 produced by carbonation had different crystal
forms. Notably, the silica gel formed by the carbonation of silicate is an amorphous substance and cannot be identified by XRD. It needs
to be further characterized in combination with other means, which will be elaborated upon in Section 3.4.2.

3.4.2. FT-IR
Fig. 10 shows the FT-IR analysis results obtained after curing for 28 days under two curing methods, and the distributions of the
different absorption bands are summarized in Table 5. The bands appearing at 1474, 857, and 712 cm− 1 may correspond to CO2− 3 in
aragonite [50,51]. The bands appearing at 1416 cm− 1 and 872 cm− 1 correspond to CO2− 3 in calcite [50,52]. The generation of these
bands under sealing curing conditions is related to the presence of CP and the small amount of calcite contained in the cement. The
band related to CO2−
3 becomes stronger under carbonation curing. The bands related to aragonite appear in samples without CP, which
is supported by the XRD results. These results indicate that carbonation results in the formation of CaCO3 polymorphs, including calcite
and aragonite.

Fig. 10. FT-IR spectra of the sealing and carbonation curing samples.

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Y.-S. Wang et al. Journal of Building Engineering 90 (2024) 109473

Table 5
FT-IR absorption wavenumbers for possible assignments and sources.

Wavenumbers (cm− 1) Assignments Sources Reference

1474 Stretching vibration (ν3) of CO2-

3 Aragonite [44]
857 In-plane bending (ν2) of CO2-3 Aragonite [50]
712 Out-of-plane bending (ν4) of CO2-3 Aragonite [51]
1416 Stretching vibration (ν3) of CO2-
3 Calcite [52]
872 In-plane bending (ν2) Calcite [53]
946 Asymmetric stretching vibration of Si–O CSH [54]
1051 Asymmetric stretching vibration of Si–O Silica gel [48]
1641 Bending vibration of O–H H2O [55]

Interestingly, the band related to Si–O bonds under sealing curing is located near 946 cm− 1 [54]. Under carbonation curing, the
peak shifts to a higher wavenumber (1051 cm− 1), which can be assigned to the Q3 or Q4 site, a typical feature of highly polymerized
silica gel [56]. After 28 days of carbonation curing, a higher degree of carbonation leads to increased polymerization of silicate chains
and decalcification of CSH into amorphous silica gel [2,48]. The absorption peak at 1641 cm− 1 corresponds to the O–H bending vi­
bration in water. Decalcification and condensation of CSH gels result in the release of water, echoing the weakening of the band related
to H–O bonds at 1641 cm− 1 [55].

3.5. Surface resistance (durability)

The use of resistivity to evaluate building material durability has been proven to be reliable in many studies [57]. Fig. 11 illustrates
the resistivity development of the seal-cured and carbonation-cured samples. CP replacement reduces the amount of cementitious
material, which may increase pore connectivity [26]. In addition, as the effective w/c increases, excess moisture benefits current
conduction. A greater number of connected pores combined with a higher water content results in a decrease in resistivity. Therefore,
at any stage of sealing curing, the greater the substitution amount of CP is, the more substantial the reduction in resistivity will be.
These results indicate that using CP to replace cement has a potential negative impact on durability when the curing condition is
sealing curing.
Under carbonation curing, the higher the CP substitution level is, the higher the resistivity, and the overall resistivity continues to
increase with the curing age. These results are due to the following two points: (1) Acceleration of carbonation curing: As described in
Section 3.1, the dilution effect of CP increases pore communication in the early curing age, reducing the diffusion resistance of CO2. CP
serves as a nucleation site for carbonation products, accelerating the development of carbonation. Studies [2,8] have noted that
carbonation curing can produce a denser microstructure and reduce the total number of pores and capillary porosity. This influence
actually changes the ion transport path in the carbonated region, enhancing the resistivity. (2) Reduction in water content: The
conduction of an electric current needs to be completed by moving ions in aqueous solution. The movement of water within the sample
toward the external environment during carbonation reduces the water content, which also enhances the resistivity. In addition, the
increase ratio in resistivity (%) at different stages of carbonation curing was calculated according to Equation (12) to analyze the effect
of CP content on resistivity.
ECPX − ECP0
E increase = × 100, (12)
ECP0

where E increase represents the increase ratio in resistivity. ECPX and ECP0 represent the resistivity of samples with different CP contents

Fig. 11. Evolution of resistivity under sealing and carbonation curing conditions.

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Y.-S. Wang et al. Journal of Building Engineering 90 (2024) 109473

and samples without CP, respectively.

Even after only a short carbonation curing period (in-molds cured for 1 d and carbonation cured for 2 d), 10 % and 20 % CP, which
are 19.6 % and 29.1 %, respectively, exhibited very obvious resistivity increases. After 7 days of curing (in-molds cured for 1 day and
carbonation cured for 6 days), the increases were the greatest, at 44.2 and 101.3 %, respectively. This result is related to the fact that
CP can promote carbonation curing. When the curing age is 28 days (in-molds cured for 1 day and carbonation cured for 28 days), the
increase ratios are 15.1 and 15.8 %, respectively. The return to a low level in the increase rate is due to the carbonated area becoming
thicker as the carbonation curing time increases. The porosity of the carbonated area is low, which delays further diffusion of CO2. The
faster carbonation of the CP sample may increase the resistivity closer to the upper limit earlier.

3.6. UPV
Fig. 12 shows the UPV development under the two curing methods. The UPV gradually increases as the curing age increases
because the products of hydration and carbonation reactions can fill the pores. After increasing the substitution level of CP, the UPV of
the mortar gradually decreased, consistent with the strength results. This result is due to the decrease in cementitious material and the
dilution effect of CP, which increases porosity.
Since the strength and UPV are affected by the internal pore size and water content, this study also performed a regression analysis
on the relationship between these two parameters under different curing methods. The results are shown in Fig. 13. A strong linear
relationship existed between strength and UPV development under sealing curing, with an R2 of 0.91. Under carbonation curing, the
linear relationship between the two parameters is slightly weaker, the data points are more discrete, and R2 is 0.80. During the
carbonation curing process, the samples were placed in an environment with a humidity of 60 %. The difference in humidity between
the inside and outside of the mortar will cause the free water inside the mortar to be lost outward. However, different carbonation
degrees and pore density also impact the rate of water loss. Therefore, the inconsistency in water content has a nonnegligible impact on
ultrasonic transmission, resulting in a weak linear correlation between strength and UPV under carbonation curing.

3.7. SEM
Fig. 14 shows the micromorphology of the samples after sealing and carbonation curing for 28 days. Fig. 13(a–c) shows that the
sealing cured cement slurries contain CH and ettringite, which have typical hexagonal flake and needle-column structures, respec­
tively. A carboaluminate phase can also be observed in the CP20–S sample (Fig. 14 (c)). It is generated by the reaction between the
carbonate ions provided by the partial dissolution of CP and the aluminum phase.
As shown in Fig. 14(d–f), the hydration products in the carbonated matrix are difficult to observe, consistent with the TG and XRD
results. Instead, an amorphous material and CaCO3 crystals with irregular shapes are produced. The precipitated CaCO3 is mainly
prism-shaped calcite and columnar microcrystalline aragonite [58]. This result is consistent with our analysis of CaCO3 precipitation
types through XRD and FT-IR. The microstructural summary showed that a good carbonation reaction of the cement matrix occurred
after 28 days of carbonation curing. Carbonation curing changes not only the composition of the material but also the microstructure,
and the material’s properties change accordingly [2,8]. Therefore, the mechanical properties and durability of the OPC-CP mortar
were improved, as discussed in Sections 3.3 and 3.5.

4. Discussion
In this study, mixtures with CP substitution levels of 0, 10 %, and 20 % were cured by sealing and carbonation. This section
discusses the mechanisms of macro- and microscale changes caused by different curing methods. The appeal of methods that involve
combining waste coral powder with carbonation curing is summarized.
Under sealing curing, CP replaces 10 % and 20 % of the cement to produce a dilution effect, which causes a reduction in the clinker
content and an increase in the effective w/c. The pores in hardened concrete correspond to the water-filled portion of the fresh slurry,
and the pore size distribution is greatly affected by the w/c. Since CP has almost no hydration activity, it cannot generate a large
amount of hydration products to fill the pores. Therefore, an increase in the effective w/c increases the pore size of the concrete. These
factors lead to material performance degradation. However, CP as CaCO3 can increase Mc and Hc in the hydration product to refine the
pores. Owing to the smaller CP particle size, there is a filler effect and a nucleation effect (for CSH), which may improve the
macroscopic properties. However, actual test results show that the dilution effect of CP dominates, decreasing the strength and re­
sistivity of the prepared mortar. This decrease in resistivity is also attributed to the increase in the effective w/c, which increases the
water content and benefits current conduction. The dilution effect of CP under sealing curing conditions decreases the performance of
concrete, which is the biggest problem restricting its widespread application in engineering [19,25].
The performance evolution mechanism under carbonation curing differs from that under sealing curing. First, after initial in-molds
curing, CP increases the porosity of the mixture through a dilution effect. Notably, under subsequent carbonation curing, an increase in
the pore size can reduce the diffusion resistance of CO2. Second, as CaCO3, CP can nucleate carbonation products [48]. The carbonation
products precipitate on the surface of the calcium-rich phase or in the internal micropores, which can give the matrix a denser
microstructure. Therefore, carbonation curing can partially compensate for the negative effects caused by the dilution effect and
improve the mechanical properties of the OPC-CP mixture. The resistivity and CP substitution level negatively correlate under sealing
curing conditions. They positively correlate under carbonation curing, and the resistivity is substantially improved. The dense pore
structure and low internal water content due to carbonation curing can limit the transport of ions from the concrete surface to the
interior. This approach has potential importance for improving the long-term durability of materials and reducing corrosion occur­
rence [59].

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Fig. 12. UPV of the mortar under sealing and carbonation curing conditions.

Fig. 13. Linear regression of compressive strength and UPV under sealing and carbonation curing conditions.

The findings of this study also revealed the importance of combining CP substitution with carbonation curing methods to improve
sustainability. (1) Clinker substitution is the most direct way to reduce the carbon footprint of concrete. The use of coral powder can
achieve this purpose and serve as a local raw material for island construction. (2) As shown in the evolution of the carbonation degree,
CP accelerates the diffusion of CO2 into the matrix, allowing the mortar to reach complete carbonation sooner. At a substitution level of
20 %, 84.4 % of the carbonation degree was reached after seven days of carbonation curing, which was 29.6 % greater than that of the
control sample. Applying this acceleration effect in practical applications can substantially shorten the carbonation curing cycle of
concrete products, allowing them to be quickly put into engineering use [59]. It also saves associated energy consumption and costs.
(3) CP can provide nucleation sites for carbonation products [48], improving the carbon sequestration efficiency. The TG results
showed that 10 and 20 % CP increased CO2 uptake by approximately 6.44 and 9.65 %, respectively. These findings demonstrate that
the combined application of carbonation curing, and CP is consistent with current concrete industry goals for improving sustainability.
However, the results are obtained according to the small samples. Owing to the size effect of carbonation curing, the carbonation
reaction can easily enter the central area of small-sized specimens; for large-scale samples, carbonation may only occur on the surface,
making it difficult to penetrate deep into the interior. Considering the large size of the concrete products produced in the project,
further verification should be carried out in practical applications.
In addition, The substitutions of CP in this study are 0, 10, and 20 %, which contrasts with the limestone powder concrete
commonly used in the engineering world. In limestone powder concrete, the maximum substitution of limestone powder is usually 20
%, so the maximum substitution of CP in this study is also 20 %. In order to distinguish it from 20 %, this study also uses the 0 % and 10
% CP. This study shows that the carbonation curing efficiency of mortar increases with the dilution effect. The study by Wang et al.
showed that the dilution effect is positively correlated with the substitution level of low-reactivity fillers [60]. For the 15 % substi­
tution, the performance is likely to be between 10 % and 20 %. For the 5 % substitution, previous researchers said that due to the
combined effect of dilution and nucleation effect under sealing curing conditions, 5 % CP concrete has a similar performance to plain
concrete [19]. Therefore, the impact of adding 5 % CP on the properties of concrete under carbonation curing conditions still needs

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Y.-S. Wang et al. Journal of Building Engineering 90 (2024) 109473

Fig. 14. Microstructure after 28 d of sealing (a, b, c) and carbonation curing (d, e, f).

experimental study. In summary, as the first step of the research, this study selected two substitution levels of 10 % and 20 % CP; in the
future, the performance of 5 % and 15 % CP concrete after carbonation curing needs to be further studied.

5. Conclusion
This study compared the effects of sealing and carbonation curing methods on cement mixtures with different CP substitution levels
(0, 10, and 20 %). The hydration kinetics, carbonation degree, strength, resistivity, and UPV development of the materials were
studied. The changes in the phase and microstructure were also analyzed. The conclusions drawn are as follows.
(1) The hydration activity of CP is extremely low. Adding it to cement causes a dilution effect, increases the effective water–cement
ratio, and reduces the 168-h cumulative heat of hydration. The normalized heat of hydration reveals that CP has a nucleating
impact, which promotes the hydration of clinker and causes the hydration peak to shift forward.
(2) Owing to the dilution effect caused by the addition of CP, the early pores increase, and the diffusion coefficient of CO2 increases;
CP can promote the precipitation of carbonation products and improve the carbonation curing efficiency of mortar. The
calculation results showed that CP with substitution amounts of 10 and 20 % increased the CO2 uptake by approximately 6.44
and 9.65 %, respectively.
(3) Phase analysis revealed that carbonation curing consumes unhydrated clinker and hydration products such as CSH, CH, and AFt
phases. It increased the CaCO3 content. FT-IR revealed that the generation of amorphous silica gel.
(4) The CaCO3 produced during carbonation curing has different crystal forms, which can be identified mainly as calcite and
aragonite through XRD and FT-IR. The SEM image shows that the matrix is well carbonized, and different crystalline phases of
CaCO3 are widely present in the matrix.
(5) Under sealing curing, CP substantially reduces the mechanical properties and resistivity. The densification effect of carbonation
curing on the matrix partially offsets the dilution effect of CP. Therefore, under carbonation curing, the reduction ratio of the
compressive strength is even lower. Furthermore, water evaporation and increased carbonation products weaken the corre­
lation between strength and UPV and increase surface resistivity.

CRediT authorship contribution statement

Yi-Sheng Wang: Writing – review & editing, Methodology, Conceptualization. Shafiq Ishak: Visualization, Formal analysis.
Guang-Zhu Zhang: Funding acquisition, Data curation. Xiao-Yong Wang: Writing – review & editing, Funding acquisition,
Conceptualization.

Declaration of competing interest

The authors declare that they have no known competing financial interests or personal relationships that could have influenced the
work reported in this study.

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Y.-S. Wang et al. Journal of Building Engineering 90 (2024) 109473

Data availability

Data will be made available on request.

Acknowledgments
This research was supported by Fundamental Research Funds for the Central Universities Science (No. 2572022DX10). This
research was supported by a National Research Foundation of Korea (NRF) grant funded by the Korean Government (MSIT) (No. RS-
2023-00208720). Yi-Sheng Wang thanks the China Scholarship Council (CSC) for financial support (No. 202308260012).

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