Construction and Building Materials 357 (2022) 129397

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Construction and Building Materials

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Effects of various curing methods on the compressive strength and

microstructure of blast furnace slag-fly ash-based cementitious material
activated by alkaline solid wastes
Weichao Guo a, b, Qingxin Zhao a, c, *, Yijia Sun a, b, Caihong Xue a, b, Yanying Bai b, d,
Yuxuan Shi b, d
a
State Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao 066000, China
b
Hebei Province Engineering Research Center for Harmless Synergistic Treatment and Recycling of Municipal Solid Waste, Yanshan University, Qinhuangdao 066000,
China
c
Hebei Province Low-carbon and Clean Building Heating Technology Innovation Center, Yanshan University, Qinhuangdao 066000, China
d
Key Laboratory of Green Construction and Intelligent Maintenance for Civil Engineering of Hebei Province, Yanshan University, Qinhuangdao 066000, China

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

Keywords: The large-scale stacking of alkaline industrial solid wastes such as soda residue (SR) and calcium carbide residue
Alkaline solid wastes (CCR) has caused serious environmental problems. Therefore, a new type of cementitious material was developed
Cementitious material in our previous study by using SR-CCR synergistically activated blast furnace slag (BFS)-fly ash (FA), which
Heat curing
abbreviated as SCBF. This paper further studied the effects of various curing methods on the compressive
Microstructure
strength and microstructure of SCBF, which was expected to provide guidance for its application in the field of
non-reinforced products such as baking-free brick. The results show that the optimal curing scheme was heat
curing at 75 ◦ C for 12 h. The optimal scheme significantly promoted an early hydration reaction and provided the
3d/28d strength values of 16.4/24.7 MPa, exceeding those of room-temperature (RT) sealed curing and water
curing by 154/24.5 % and 264/31 %, respectively. Besides, the optimal scheme accelerated the formation of
C–S–H gel, Hydrotalcite (6MgO⋅Al2O3⋅CO2⋅12H2O), Hydrocalumite (3CaO⋅Al2O3⋅CaCl2⋅10H2O), and other
crystal products, as well as increased the consolidation rate of chlorine ion from 37.9 % (in RT sealed curing) to
64.3 %. These hydration products were evenly distributed, effectively filling the pores and reducing the mac­
roporosity from 9.30 (in RT sealed curing) to 1.54 %, thus improving the early and later-age strength. Too high
curing temperature (exceeding 75 ℃) or prolong heat curing period (exceeding 12 h) would cause microstructure
deterioration, significantly increase the number of macropores and microcracks in the matrix, ultimately leading
to strength retrogression.

1. Introduction extensive research efforts [2]. Besides, this hydraulic cementitious ma­
terial’s production implies the utilization of waste precursor materials
Cement is a world champion among construction materials by (industrial solid wastes such as fly ash (FA), steel slag, red mud, phos­
popularity and application scope. However, its production process of phorus slag, blast furnace slag (BFS), etc.), which can effectively reduce
“two grinding and one burning” (raw meal grinding → clinker calcina­ environmental pollution caused by these solid wastes [3]. It has been
tion → cement grinding) is characterized by high energy consumption reported that the resulting AACMs exhibit excellent durability perfor­
and high pollution, as well as depends on limited natural resources of mance [4–7].
limestone. Therefore, the development of more sustainable and low- The various performances of BFS and FA precursor materials under
carbon alternative materials became quite topical [1]. As a potential the action of strong alkali (sodium hydroxide, water glass, etc.) activa­
cement replacement with substantial advantages of low energy con­ tors have been explored a lot [8]. Strong alkali activation was found to
sumption and low CO2 emission, the alkali-activated cementitious ma­ be too expensive and inducing too fast setting [9], which restricted its
terial (AACM) presently enjoys global attention and is a focus of mass implementation and application scope. Alternatively, some

* Corresponding author at: State Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao 066000, China.
E-mail address: [email protected] (Q. Zhao).

https://doi.org/10.1016/j.conbuildmat.2022.129397
Received 17 July 2022; Received in revised form 24 September 2022; Accepted 6 October 2022
Available online 13 October 2022
0950-0618/© 2022 Elsevier Ltd. All rights reserved.
W. Guo et al. Construction and Building Materials 357 (2022) 129397

alkaline industrial solid wastes were recently used to activate BFS or FA was clarified, and the optimal curing scheme was determined. The
and prepare the cementitious material, yielding good results on the research results can promote the application of SCBF in the field of
setting time extension and cost reduction. The waste alkali contained in unreinforced products such as baking-free bricks, and reduce the envi­
the alkaline solid wastes can replace the strong alkali as the activator. ronmental pollution of such industrial solid wastes as SR and CCR.
Calcium, silicon, aluminum, and other components can be used as pre­
cursor supplements, thus achieving a dual effect. Soda residue (SR) and 2. Experimental program
calcium carbide residue (CCR) are alkaline industrial wastes discharged
in the soda ash production by ammonia alkali process and acetylene gas 2.1. Raw materials
production by hydrolysis of calcium carbide, respectively [10–12]. In
China, the annual output of SR and CCR reaches 7.8 [13] and 30 million Soda residue (SR), calcium carbide residue (CCR), blast furnace slag
tons [14], respectively. Due to limited waste utilization options and (BFS), fly ash (FA), and sand are the main raw materials. Both SR and
capability, they are mostly piled up in the open air, occupying vast land CCR raw materials were initially in slurry state, and they should be
resources and polluting the soil, groundwater, and air. SR and CCR are dried, ground, and sieved to test the chemical and phase compositions.
discharged in the form of slurry, with a wet base pH of 11,12 and 12,13, The chemical compositions of SR, CCR, BFS and FA were identified by X-
respectively, which strong alkalinity allows one to use them as alkali ray fluorescence (XRF) experiments, whose results are listed in Table 1.
activators. Thus, Lin et al. [15] and Zhao et al. [16] prepared new The phase compositions were determined by X-ray diffraction (XRD)
cementitious materials with SR to activate BFS, Zhang et al. [17] and Li experiments, and a D/MAX-2500/PC X-ray diffractometer was
et al. [9] used CCR to activate BFS, while Dueramae et al. [18] and employed with a voltage of 40 kV, a current of 40 mA, a scanning angle
Namarak et al. [19] applied CCR to activate FA. The respective hydration of 5-65◦ , and a scanning rate of 2◦ /min. The XRD results are plotted in
and hardening mechanisms were revealed by microstructure examina­ Fig. 1.
tion via SEM, XRD, and TG-DSC. However, the early strength of these SR and CCR’s initial water content were determined by oven drying
cementitious materials was found to be quite low. In particular, the 7d method, and both exceeded 90 %. Before use, they were left for 5–7
strength of SR-BFS and CCR-FA mortar samples was less than 5 MPa, days, with daily removal of the supernatant and mixing of the deposited
suggesting that the alkali activation of SR and CCR mainly occurred at layers; when the water content of the deposited layer was reduced to
later stages of the cementitious material aging process. Guo et al. [20] 40–60 %, the obtained slurry samples were used as activators. This
prepared quaternary cementitious materials with multiple strength direct use of slurry can reduce the energy consumption of drying and
grades (15–40 MPa) by optimizing the proportion of SR and CCR and grinding processes. According to the application method of the slurry
using them as composite activators to activate BFS-FA, which further proposed in our previous study [32], the functional relationship be­
expanded the scope of application. However, at FA content exceeding tween the slurry density (ρ, g/cm3) and solid content (S, %) was first
25 %, the early strength was still low. established, as shown in Eqs. (1), (2). In application, the slurry density
By optimizing the curing methods, one can improve the early me­ can be directly measured to calculate the solid content, and then the
chanical properties of cementitious materials. The available optimized required slurry mass can be inversely calculated from the dry basis mass.
curing methods include heat curing [21], steam curing [22], autoclave
SR : Ys = 37.920ρs − − 22.777 (1)
curing [23], microwave curing [24–25], etc. Compared with other
curing methods, heat curing is easier to operate. Also the optimal heat
CCR : Yc = 128.922ρc − − 121.223 (2)
curing can improve the cementitious material’s microstructure, me­
chanical properties, and durability [26–27], it has become the research The main components of SR were CaO, Cl and SiO2 (Table 1), and
−

interests. The sensitivity of different activators and precursors to tem­ the main phases were Halite (NaCl) (PDF#99-0059), Gypsum
perature is different, and the mechanical properties vary with heat (CaSO4⋅0.5H2O) (PDF#81-1849), Calcium chloride hydroxide (CaClOH)
curing parameters, being related to the properties and the ratio of raw (PDF#73-1885), and Calcite (CaCO3) (PDF#88-1807) (Fig. 1). The main
materials. However, in most cases, the heat curing parameters can be components of CCR were CaO (Table 1), and the main phases were
optimized. According to previous research, the appropriate curing Calcite, Portlandite (Ca(OH)2) (PDF#72-0156) and Hydrocalumite
temperature range for the AACM is 25–120 ◦ C, and the optimal curing (3CaO⋅Al2O3⋅CaCl2⋅10H2O) (PDF#31-0245) (Fig. 1).
time is 2–48 h [26–30]. Nasir et al. [26] found that a 60 ◦ C curing for 6 h The selected S95 grade BFS comprised such main components as
was the optimal curing scheme for NaOH-Na2SiO3 activated BFS-silico- CaO, SiO2, and Al2O3 (Table 1), while Quartz (SiO2) (PDF#79-1906)
manganese fume binder, under which the 3d strength reached 83.6 % of was its main phase (Fig. 1). The obtained XRD pattern featured a pro­
28d one, and then the strength growth rate slowed down. Namarak et al. nounced hump between 20 and 40◦ , indicating that it contained a lot of
[19] developed FA-CCR cementitious material and reported that the amorphous material [26]. The F.II grade FA was selected, which main
increase of curing temperature was conducive to the development of components were SiO2 and Al2O3, (Table 1) and the main phases were
early strength, but harmful to the later strength. Salih et al. [27] studied Quartz and Mullite (3Al2O3⋅2SiO2) (PDF#79-1275) (Fig. 1). The mean
the alkali-activated palm oil fuel ash binder, and found that the alkali- particle size of BFS and FA are 14.66 and 12.36 μm respectively, the
activated reaction at a 70 ◦ C curing was sufficient to achieve a high
degree of geological polymerization and increase the early and late Table 1
strength values. Jaarsveld et al. [31] revealed that the curing tempera­ Chemical composition (wt.%) of materials.
ture had a negligible effect on the crystalline phase transformation of Oxide SR CCR BFS FA
alkali activated FA binder, affecting only the gel products of the amor­
SiO2 9.87 4.68 32.6 46
phous phase in the structure.
Al2O3 3.25 2.96 17.1 41.6
Overall, there are multiple research results on optimizing curing CaO 43.2 90 33.7 5.25
methods for strong alkali-activated cementitious materials, but the MgO 9.77 0.23 7.96 0.23
respective data on alkaline solid waste-activated cementitious materials Fe2O3 0.91 0.2 1.18 2.91
are scarce. Therefore, based on our previous research findings [20], we MnO – – 0.31 1.31
TiO2 0.12 0.11 2.54 1.48
attempt in this paper to optimize the curing methods for the developed K2O 0.29 – 0.57 0.92
SR-CCR activated BFS-FA cementitious material (SCBF) with low early SO3 5.57 0.65 3.21 0.64
strength. According to the experimental results of compressive strength Na2O 3.93 0.3 0.56 0.33
evolution and microstructural features under different curing methods, Cl− 23 0.78 – –
Loss on ignition 2.86 4.25 2.14 1.57
the influence mechanism of curing methods on the compressive strength

2
W. Guo et al. Construction and Building Materials 357 (2022) 129397

7 1- Calcium Chloride Hydroxide

2- Gypsum 5- Portlandite
3- Halite 6- Hydrocalumite
4- Calcite 7- Quartz
888 7 8 8- Mullite
7
FA 8 7 8 8

GGBS 7
intensity (a.u.)

5
5

6 5 5 5
CS 4 5
2 55
2
3 3
2 14 1
SR 1 1 1 2
11

5 10 15 20 25 30 35 40 45 50 55 60 65
Fig. 3. Sample preparation process and curing scheme (RT = Room tempera­
2
ture, 20–25 ◦ C).
Fig. 1. XRD diffractogram of raw materials.
sand-binder was 3.0. The preparation process, curing scheme and
experimental items are depicted in Fig. 3.
The mechanical properties of SCBF were characterized by the mortar
compressive strengths. The chloride ion consolidation rate was tested
using the mortar fragments. The sand-free paste samples were adopted
for the microscopic tests. When preparing samples, the water contained
in the SR and CCR slurry need to be included in the total water con­
sumption, and the insufficient water amount was compensated by tap
water. After the mortar or paste was mixed evenly, half of the sample
was put into the test mold firstly, vibrated for 60 times, then the
remaining sample was put into the test mold, vibrated for 60 times, and
finally scraped using a flat plate. The samples were sealed at room
temperature (RT, 20–25 ◦ C, relative humidity ≥50 %) for 24 h before
demoulded. Then, according to the curing scheme in Fig. 3, the S1
sample was placed in the water for curing (20 ± 1 ◦ C); the S2 one was
placed at RT for dry curing; the S3 sample was sealed and cured at RT;
the S4-10 samples were first sealed for heat curing, and then transferred
to RT to continue sealed curing.

2.3. Method
Fig. 2. Particle grading curves of river sand.
The compressive strength test was conducted according to GB/T
specific gravity are 2.74 and 2.45 respectively, and the specific surface 17,671 (China standard) [33]. Cuboid mortar samples of 40 mm × 40
area are 419.5 and 472.4 m2/kg. mm × 160 mm dimensions were used to test the compressive strength at
The river sand with particle size of 0.08–5.0 mm was used as fine 3, 7, 28, 56d. The mean value and standard deviation of three samples
aggregate, whose particle grading curve is shown in Fig. 2, indicating characterized the results.
that it belonged to medium sand in zone II. The apparent and bulk The Cl− consolidation rate test was conducted according to JGJ/T
densities were 2750 and 1540 kg/m3, respectively, the fineness modulus 322 (China standard) [34]. The calculation formula is as follows:
was 2.86, and the mud content was 1.8 %. A A
WCl − WCl
(3)
−
W= A
× 100%
WCl −

2.2. Sample preparation

where W—Consolidation rate of Cl− (%).
A
Previous research results [20] show that the 28-day strength of SCBF WCl − —The percentage of total Cl
−
in the raw materials to the mortar
ranged from 17.5 to 43.2 MPa for different proportions of BFS and FA. At mass (%).
w
high FA content, its early strength was low, and its application was WCl - —The percentage of water-soluble Cl to the mortar mass (%),
−

limited. Therefore, this study envisaged improving the mechanical which can be obtained through experiments.
properties of the SCBF with high content of FA through heat curing. The The microstructural examinations were performed using cylindrical
mix ratio was based on the mass percentage of dry base and implied SR: paste samples with Φ40 mm × 60 mm dimensions. Before the test, the
CCR: BFS: FA = 25:5:30:40, the water-binder ratio was 0.5, and the samples were broken into blocks, dried in the isopropanol via the

3
W. Guo et al. Construction and Building Materials 357 (2022) 129397

solvent-replacing drying method [35], and the hydration was stopped. early and late strength improvements were significant and slight,
Then, a vacuum dryer was used to remove the isopropanol by contin­ respectively.
uous volatilization. For the XRD, FTIR, and TG tests, samples were
ground into powder and sieved with a 0.075 mm square hole sieve. The Possibly, the appropriate heat curing accelerated the hydration re­
SEM and MIP tests were conducted on blocks with side lengths less than action of the SCBF, so more hydration products were formed in the
10 mm. Other microscopic experimental parameters are shown in system, enhancing its structural compactness and strength [36]. How­
Table 2. ever, a too high curing temperature will cause the strength drop, as
reported in previous studies [27,29]. There two possible explanations of
3. Results and discussion this phenomenon: (i) the gel products rapidly produced by heat curing
will encapsulate some precursor particles and impede their hydration
3.1. Compressive strength of mortar samples reaction [27], and (ii) heat curing leads to rapid gel formation with
nonuniform distribution, which is favorable for the appearance of wide
Fig. 4 shows the test results of compressive strength under different cracks and pores in the hardening structure that would reduce its
curing methods and various heat curing temperatures. Fig. 5 shows the strength [37]. It should be emphasized that heat curing was more
test results of compressive strength at a curing temperature of 75 ◦ C and effective in improving the early strength, while in the later period (after
different heat curing periods. 28 days), the strength difference between heat curing and water curing
was significantly reduced, which may be due to the fact that the hy­
3.1.1. Effects of curing method and heat curing temperature on the dration degree under long-term water curing was gradually close to that
compressive strength under heat curing.
According to Fig. 4, water-cured samples with lowest compressive
strength values were observed at 3/7d ages (4.4/10.1 MPa, respec­ 3.1.2. Effects of heat curing period on the compressive strength
tively). In comparison, the 3/7d strength values of RT dry-cured and According to Fig. 5, at a curing temperature fixed at 75 ◦ C and a
sealed cured samples were 5.3/12.2 MPa and 6.1/13.1 MPa, respec­ curing period extended from 6 to 24 h, the 3d compressive strength
tively (being higher by 20.5/20.8 % and 38.6/29.7 %). When the curing sharply grew by 37.8 % in the interval from 6 to 12 h (i.e., from 11.9 to
age was prolonged to 28/56d, the strength of water cured and RT sealed 16.4 MPa). When curing period was prolonged from 12 to 24 h, the
cured samples grew steadily to 20.4/23.2 and 22.6/24.9 MPa, respec­ compressive strength increased slightly to 16.8 MPa (18 h) and then
tively, with negligible difference between the two. However, the dropped to 16.6 MPa (24 h). At 7d, 28d, and 56d, the compressive
strength of RT dry-cured samples exhibited a slight growth to 14.1/14.7 strength first increased and then dropped with curing period, and the
MPa, with saturated development of late strength. This could be highest strength was obtained at a curing period of 12 h. Overall, 12 h
attributed to the rapid water dispersion in the dry state at room tem­ was the optimal curing period: higher values will cause the late strength
perature, leading to the insufficient hydration reaction due to the lack of to decrease, as confirmed by some previous research results [26,38]. It is
water supply in the later stage. Meanwhile, the RT sealed curing pre­ generally believed that the gel product will shrink and produce more
vented water loss, providing a sufficient water content in samples for the cracks after a long time of heat curing, resulting in the late strength
later hydration reaction and continuous strength development. decline [38–39].
With an increase in curing temperature, the compressive strength
exhibited the following trends: 3.2. Consolidation rate of chloride ions

1) From RT to 75 ◦ C, the compressive strength of mortar samples at all SR and CCR raw materials contain chloride ions (Cl− ), which can
ages grew, especially at 3d, with the strength increase from 6.1 to participate in the hydration reaction, mainly producing the
16.4 MPa (i.e., by 168.9 %). At the ages of 7/28/56d, the strength 3CaO⋅Al2O3⋅CaCl2⋅10H2O crystals. Besides, some Cl− can be solidified in
values grew from 13.1/22.6/24.9 MPa to 19.7/24.7/26.6 MPa (by the C–S–H gel. Therefore, the hydration process with Cl− can be
50.4/9.3/6.8 %), and the strength increment decreased with age. characterized by testing the consolidation rates of Cl− for different
2) With a curing temperature increase from 75 to 90 ◦ C, the compres­ curing methods and sample ages. The representative mortar samples of
sive strength of samples at all ages decreased slightly, from 16.4/ water curing (S1), RT sealed curing (S3), heat curing of 75 ◦ C for 12 h
19.7/24.7/26.6 MPa to 15.2/17.2/20.6/22.1 MPa, respectively. (S6), 90 ◦ C for 12 h (S7), and 75 ◦ C for 24 h (S10) were selected to test
According to the above strength development trend, the optimal heat the Cl− consolidation rate at the age of 3-56d. The results are plotted in
curing temperature was 75 ◦ C, and its 3d strength could reach 66.4 % Fig. 6.
of the 28d strength. Compared with normal temperature curing, the The Cl− consolidation rate of samples cured at RT(sealed) was the
lowest at the ages of 3d and 7d (37.9 and 44.4 %, respectively). The Cl−
consolidation rate of samples with water curing was slightly higher, but
Table 2 this effect could be provided by the partial diffusion of Cl− in the curing
Microscopic experimental parameters.
water rather than by the respective reaction. After the early curing
Item Experimental instrument Experimental parameters Sample temperature rose to 75 and 90 ◦ C, the 3d and 7d Cl− consolidation rates
age
reached 64.3 and 69.0 % versus 69.6 and 70.2 %, respectively. This
XRD D/MAX-2500/PC X-ray Voltage: 40 kV; Current:40 mA; 3, 28 d implies that the heat curing significantly promoted the hydration reac­
diffractometer Scanning rate: 2◦ /min; Scanning tion, accelerated the formation of chlorinated hydrated products, and
angle: 5-65◦ .
FTIR E55＋FRA106 Fourier Wavenumber range: 4000–400 3, 28 d
cured more Cl− . After the curing period was prolonged from 12 to 24 h,
infrared spectrometer cm− 1; Resolution: 2 cm− 1 the 3d and 7d Cl− consolidation rates reached 66.1 and 69.8 %,
TG STA449C/6/G Protective gas: Ar; Temperature 3d respectively, implying that the increased curing period slightly pro­
comprehensive thermal range: RT-1000 ℃; Heating rate: moted the early hydration reaction.
analyzer 10 ◦ C/min
At 28d, the Cl− consolidation rate of samples with RT sealed curing
SEM TESCAN-VEGA3 Accelerating voltage: 5–10 kV; 3d
scanning electron Work distance: 10–12 mm; and water curing sharply grew from 44.4 and 49.6 % to 71.9 and 75.4 %,
microscope Magnification: 2000 respectively, which indicates that they experienced more intensive hy­
MIP AutoPore IV 9500 Pore size range: 3–350000 nm; 28 d dration reaction in 7–28 d, promoting the Cl− curing. However, the Cl−
automatic mercury Mercury surface tension: 0.485 N/ consolidation rate of three groups of heat curing samples grew only
porosimeter m; Contact angle: 130◦
slightly because the heat curing accelerated the early hydration reaction

4
W. Guo et al. Construction and Building Materials 357 (2022) 129397

3d 7d 28d 56d
30
26.6
24.9 24.7
25 23.2 23.6
Compressive strength (MPa) 22.6 21.9 22.1
20.8 21.4
20.4 20.6
19.7
20
17.2
16.4
15.9
15.2
14.114.7 13.9
15 13.1
12.2 12.5

10.1
10 8.9

6.1
5.3
5 4.4

0
Water RT RT (Sealed)
Curing type
Fig. 4. Effects of curing method and heat curing temperature on compressive strength.

Fig. 5. Effect of heat curing period on compressive strength.

Fig. 6. Curing method effect on chloride ion consolidation rate.
but inhibited the later hydration reaction. Overall, the consolidation
rate of Cl− was the highest after heat curing at 75 ◦ C for 12 h, reaching 3.3. Characterization by X-ray diffraction
76.6 and 80.7 % for 28d and 56d ages. A too high curing temperature
(90 ◦ C) or excessive curing period (24 h) decreased the Cl− consolidation Typical S1, S3, S6, S7, and S10 samples were subjected to the XRD
rate in the late period, which was consistent with the strength devel­ examinations, and the 3d and 28d test results were obtained and plotted
opment trend. This may be because excessive heat curing induced more in Fig. 7(a) and (b), respectively. The number near the characteristic
pores and cracks in the gel matrix, which harmed Cl− curing. peak represents the intensity value, so that each group can be compared
It should be emphasized that solid waste products are used in various conveniently.
scenarios, the leaching requirements of Cl− are different, and the test Six main crystal phases were identified in the spectrum: Hydro­
methods are also different. The SCBF studied in this paper was mainly calumite (3CaO⋅Al2O3⋅CaCl2⋅10H2O, HC) (PDF#31-0245) and Hydro­
used to prepare baking-free bricks, and there is no unified evaluation talcite (6MgO⋅Al2O3⋅CO2⋅12H2O, HT) (PDF#41-1428) were the main
standard for chloride ions’ leaching rate in this field. Therefore, in crystal products formed by the hydration of BFS-FA under synergistic
practical application, the Cl− leaching requirements of different sce­ alkali activation of SR-CCR. Other crystals mainly came from raw ma­
narios should be considered to determine whether the cementitious terials or carbonization, including Quartz (SiO2) (PDF#79-1906),
material is suitable. Mullite (3Al2O3⋅2SiO2) (PDF#79-1275), Halite (NaCl) (PDF#99-0059)
and Calcite (CaCO3) (PDF#88-1807).
As shown in Fig. 7(a), at the age of 3d, a significant phase change was
indicated by the characteristic peaks of Quartz (at 2θ = 26.6◦ ), HC/HT

5
W. Guo et al. Construction and Building Materials 357 (2022) 129397

A-Calcium chloroaluminate hydrate S-Hydrotalcite C-Calcite H-Halite

Q-Quartz M-Mullite

S/A 826
H 3 days
946 MQ A 801
S C
598 A M MM H
M
1048 M A AA M
AA M
773 852
622

949
intensity (a.u.)

874 811
605

969
821 719
574
RT (sealed)

989
743 674
541
Water

5 10 15 20 25 30 35 40 45 50 55 60 65
2 (a)

H 28 days
S/A 963 803
M Q C A 786
S M
592 A MM M H
M A AA
1077 AA M M
771 861
632

988
intensity (a.u.)

816
736
612
1110

801
754
583
1004 RT (sealed)

767 792
554
Water

5 10 15 20 25 30 35 40 45 50 55 60 65
2 (b)
Fig. 7. XRD patterns of 3d (a) and 28d (b) samples.

(at 2θ = 11.2◦ ), HC (at 2θ = 23.4◦ , 31.1◦ ), and HT (at 2θ = 22.6◦ ). significantly, indicating that heat curing also promoted the formation of
Taking the water-cured samples as the reference, the Quartz charac­ HC and HT crystals. When the curing period was prolonged from 12 h to
teristic peak intensity (CPI) of samples with RT sealed curing was 24 h, the CPI of Quartz decreased, while those of HC and HT remained
approximately equal. In contrast, the CPIs of HC and HT were slightly unchanged. This implies that the increased heat curing period continued
enhanced, indicating that the RT sealed environment was conducive to to promote the dissolution of the Quartz phase to generate C–S–H, but
the formation of HC and HT crystals. After the early curing temperature it had little effect on the growth of HC and HT crystals.
rose to 75 and 90 ◦ C, the Quartz CPI drastically dropped, possibly due to According to Fig. 7(b), at 28d, the crystal phases of specimens with
Quartz phase dissolution in BFS/FA accelerated by heat curing, forming water curing and RT sealed curing changed the most, the CPI of Quartz
active silicon, promoting the C–S–H gel formation, and enhancing at 2θ = 26.6◦ was significantly lower than that at 3d, in contrast to those
strength [27,29]. Additionally, the CPIs of HC and HT also increased of HC/HT at 2θ = 11.2◦ and HC at 2θ = 31.1◦ , which were significantly

6
W. Guo et al. Construction and Building Materials 357 (2022) 129397

increased, exceeding that of samples with heat curing at the same age. The bands near 453, 530, 801, 974, 1090 cm− 1 in Fig. 8 can be
The above results show that the samples under these two curing methods attributed to the vibrations of Si-O bond, indicating the presence of
experienced more intensive hydration reactions in 3–28 d, and the hy­ C–S–H gel [9,40–42]. Among them, the bands near 1090 cm− 1 do not
dration products of the C–S–H gel, HC and HT crystals, increased have a significant regularity due to their low intensity, but the other four
significantly. The Quartz CPI of the sample cured at 75 ◦ C for 12 h was bands show a significant variation regularity. At 3d, these four CPI
slightly lower than that of 3d. The HC and HT CPIs increased slightly, values has little difference between samples cured in water and RT
indicating that a slower hydration reaction occurred in 3–28 d. How­ sealed, but they sharply grew when the early curing scheme was
ever, the XRD patterns of specimens cured at 90 ◦ C for 12 h and 75 ◦ C for changed to the optimal heat curing (75 ◦ C@12 h). It represented that the
24 h had little changes compared with those of 3d. Only the Quartz CPI transmittance of Si-O bond was significantly reduced, and the produc­
decreased slightly, and those HC and HT remained nearly unchanged, tion of C–S–H gel increased significantly [43–44]. When the curing
indicating that Quartz still dissolved to form C–S–H in the later stage temperature rose to 90 ◦ C or the heat curing period was extended to 24
of samples with excessive heat curing, while the HC and HT crystals h, these CPI values further increased, indicating that the amount of
mainly grew in the earlier stage and remained almost unchanged in the C–S–H gel continued to grow. When the curing age was extended to
later stage. 28d, these CPI values were further enhanced under all curing methods,
Besides, the Calcite CPI under heat curing significantly exceeded proving that the formation of C–S–H gel increased with age. However,
those under RT sealed curing and water curing. It increased with age, the amounts of C–S–H formed under normal temperature curing were
indicating that the heat effect on the Ca(OH)2 carbonization continued still less than that of heat curing. The above results show that proper
with aging. Under all curing methods, the Mullite CPI in the 3d and 28d heat curing can significantly promote the hydration reaction and in­
patterns changed negligible, which implied that the Mullite crystals of crease the production of C–S–H gel in the early and late stages. This
FA did not participate in the hydration reaction. may be the main reason for increased values of early and late strengths.
The absorption peaks near 3435 and 1638 cm− 1 can be attributed to
the stretching and bending vibrations of H–O–H bond, respectively
3.4. FTIR spectroscopy analysis
[45–46], mainly caused by hydroxyl groups in the C–S–H gel and the
HC [47]. Through comparison, it can be seen that the change in the
FTIR tests were carried out on S1, S3, S6, S7, and S10 samples, and
H–O–H absorption band for 3d and 28d ages was similar to that of the
the 3d and 28d test results were obtained and plotted in Fig. 8.
Si-O. This further indicates that suitable heat curing can improve the
formation of the C–S–H gel and the HC crystal.
3435 1638
1440 875 453 The bands near 1440 and 875 cm− 1 were caused by the vibrations of
801
974 530 C–O bond in the Calcite and HT [48–49]. At the age of 3d, compared
with water curing, these two CPIs increased slightly at RT sealed curing
and further grew when the curing temperature rose to 75 and 90 ◦ C. In
contrast, the CPI remained unchanged when the curing period was
Transmittance (a.u.)

prolonged to 24 h, which shows that proper heat curing accelerated the

formation of Calcite and HT. At the same time, too long curing times had
a negligible effect on the change of the two crystalline phases. At the age
RT (sealed) of 28d, these two CPIs were further enhanced in all samples because the
Ca(OH)2 in the matrix was carbonized further with age, which was
consistent with the XRD findings.
Water 1090

3.5. Thermogravimetric (TG) analysis

To further characterize the effects of various curing regimes on the

3 days
early hydration products of SCBF. TG tests were carried out on S1, S3,
4000 3500 3000 2500 2000 1500 1000 500 S6, S7, and S10 samples. The TG-DTG curves of 3d age and the weight
Wavenumber (cm-1) (a) loss statistics for temperature ranges of 50–200 ◦ C, 250–400 ◦ C, and
750–950 ◦ C are plotted in Figs. 9 and 10, respectively.
3435 1638
1440 875 453
In Fig. 9, three pronounced weight loss peaks can be observed. The
974 801 530
weight loss of 50–200 ◦ C corresponds to the dehydration-induced
1090
decomposition of the C–S–H gel [17,50]. The weight losses of the
five groups of samples were 4.72, 5.19, 6.18, 6.67, 6.56 %, respectively,
and the weight loss gradually increased. From RT to 75 ◦ C, the weight
Transmittance (a.u.)

loss increment was the largest, which implied that suitable heat curing
could significantly promote the C–S–H gel production. However, from
75 ◦ C to 90 ◦ C or from 12 h to 24 h at 75 ◦ C, the weight loss increased
RT (sealed) only slightly, indicating that excessive heat curing had a weakened
promotion effect on hydration reaction. The weight loss at 250–400 ◦ C
was caused by dehydration of HC and HT [47,51]. The weight losses of
Water five groups of samples in this temperature range were 3.14, 3.21, 3.68,
3.85, and 3.74 %, respectively, and the weight loss increased signifi­
cantly from RT to 75 ◦ C, indicating that the optimal heat curing signif­
icantly promoted the formation of HC and HT crystal products. Still, the
28 days productivity changes were negligible after the optimal curing temper­
4000 3500 3000 2500 2000 1500 1000 500 ature and time were exceeded. The Calcite decomposition caused the
Wavenumber (cm-1) (b) weight loss peak at 750–950 ◦ C [52]. The weight losses of five groups of
samples in this temperature range were 2.13, 2.51, 3.05, 3.17, and 3.01
Fig. 8. FTIR curves of 3d (a) and 28d (b) samples. %, respectively. The minimal amount of Calcite was formed under water

7
W. Guo et al. Construction and Building Materials 357 (2022) 129397

100 1.5
TG 1.2
95
0.9
90
DTG 0.6
85 0.3
TG (%)

80 0.0

-0.3
75 FS / HT
Water Calcite -0.6
70 RT (sealed)
-0.9
65 C-S-H
-1.2

60 -1.5
100 200 300 400 500 600 700 800 900
Temperature (°C)
Fig. 9. TG-DTG curves of 3d samples.

of the two samples. When the early curing scheme was changed to the
optimal heat curing (75 ◦ C@12 h), the number of unreacted particles on
the surface sharply dropped, and more C–S–H gel were generated,
which continuous distribution significantly increased the paste
compactness. This indicates that suitable heat curing can significantly
promote the hydration reaction, accelerate the gel formation, and
rapidly enhance the strength. When the curing temperature rose from 75
to 90 ◦ C, some gel particles appeared. Still, most of them were dispersed,
had less continuous and uniform distribution, and there were wide
cracks and holes in many locations. Similar phenomena were observed
in previous studies [26,53]. When the heat curing period was prolonged
to 24 h, despite the formation of more continuous C–S–H gel,
shrinkage cracks appeared in some gel matrices, consistent with findings
of previous studies [38–39]. In summary, when the curing temperature
was too high or the heat curing period was too long, more cracks or holes
were produced in the microstructure. These initial defects may be the
main reason for the late strength reduction.

3.7. Pore structure analysis

Fig. 10. Weight loss of 3d samples at different temperature range. To characterize the effect of various curing schemes on the pore
structure of paste, mercury intrusion porosimeter (MIP) tests were
conducted on S1, S3, S6, S7, and S10 samples of 28d. The cumulative
curing because water-cured samples had less chance of contacting CO2,
distribution curves and differential distribution curves of pore structures
and the carbonation was reduced during the hydration process. The
of all samples were presented in Fig. 12 and Fig. 13, respectively. Then,
amount of Calcite formed under RT sealed curing increased slightly,
according to [54], all pores were classified into mesopores (medium-
while that under heat curing increased significantly, indicating that heat
sized pores, 3–50 nm), macropores (large-sized pores, 50–10000 nm),
curing significantly promoted the carbonation of Ca(OH)2. These find­
and voids/microcracks with pore diameters exceeding 10000 nm. The
ings further confirmed the XRD and FTIR test results.
results of pore size classification and total porosity are presented in
Table 3.
3.6. Characterization by scanning electron microscope Compared with water curing, the porosity of all kinds of pores
decreased slightly under RT sealed curing, and the total porosity drop­
To characterize the effects of various curing schemes on the early ped from 23.50 to 21.35 %. The pore size distribution curves of the two
micromorphology of SCBF, SEM tests were carried out on S1, S3, S6, S7, were relatively close. When the early curing scheme was changed to the
and S10 samples at the age of 3d. The results can be seen in Fig. 11. optimal heat curing (75 ◦ C@12 h), the porosity further decreased from
There was little difference in the micromorphology between the 21.35 to 18.44 %, the pore diameter distribution curve shifted to the low
samples cured by water and sealed at RT. The cross-section contained pore diameter direction, the number of mesopores was increased by
numerous debris, and the microstructure was loose. More unreacted raw 41.9 %, and the number of macropores dropped by 83.4 %. This was
material particles could be observed, reflecting a low hydration degree because the optimal high-temperature curing promoted the formation of

8
W. Guo et al. Construction and Building Materials 357 (2022) 129397

Fig. 11. SEM images of 3d-cured samples: (a) water curing, (b) RT(sealed) curing, (c) 75 ◦ C for 12 h, (d) 90 ◦ C for 12 h, (d) 75 ◦ C for 24 h.

gel and crystal products, thereby effectively filling pores between the temperature was raised to 90 ◦ C, the total porosity jumped from 18.44 to
particles and making the microstructure more compact. The excellent 38.35 and 32.41 %, respectively, with a slightly increased number of
pore diameter distribution also contributed to higher late strength. mesopores and greatly increased the number of macropores, voids, and
When the heat curing period was prolonged to 24 h at 75 ◦ C or the curing microcracks. This indicates that excessive high-temperature curing
promoted the formation of macropores, voids, and microcracks. Even if
the formation of gel products were promoted simultaneously, the later
0.35 strength would be deteriorated by microcracks. This finding further
verifies the SEM test results.
0.30
Cumulative Intrusion V (ml/g)

Water 3.8. Discussion

0.25 RT(sealed)
By summarizing the above test results, the early microstructure
0.20 development of the SCBF under different curing methods was plotted in
Fig. 14.
0.15 The optimal heat curing (12 h at 75 ◦ C) significantly promoted the
early hydration reaction. It provided rapid and steady formation of the
C–S–H gel, HC, HT, and other crystals. More gel would be continu­
0.10 ously distributed, and the crystal products would fill the pores, reducing
the porosity, significantly improving the early strength, and slightly
0.05 enhancing the late one. At too high a curing temperature (12 h at 90 ◦ C),
the gel product is formed too fast, leading to its insufficient dissolution,
0.00 transfer, and precipitation, as well as rapid stacking and wrapping on the
1 10 100 1000 10000 100000 precursor particles, thus hindering the later hydration reaction of the
Pore diameter (nm) precursor. This results in dispersive distribution of the gel and the for­
mation of wider cracks and holes, reducing the late strength. Under
Fig. 12. Cumulative distribution curves of pore structures. excessive heat curing time (24 h at 75 ◦ C), although the hydration

9
W. Guo et al. Construction and Building Materials 357 (2022) 129397

In general, the growth and evolution of gel products are the key
factors controlling the early strength of the SCBF. As to the effects of the
crystal products on the cementitious material’s mechanical properties,
several researchers reported contradicting results for various cementi­
tious materials. For example, Nasir et al. [26] proved that the growth of
Quartz crystals in the alkali-activated BFS-silico-manganese fume binder
strongly contributed to the strength development under heat curing. In
contrast, Salih et al. [27] and Tian et al. [29] reported that heat curing
had a slight effect on the crystal phase change, so the effect of the crystal
on the cementitious material’s strength was negligible. In this study, the
behavior of HC, HT, and Calcite crystals significantly changed with the
curing temperature and time. The growth of HC crystals has a micro-
expansion effect [55–56], providing the filling of pores, and was
considered beneficial to strength development [57]. The HT crystals has
the potential to improve durability due to its unique layered structure
and ion adsorption capacity, which can adsorb Cl− ,SO2− 4 , etc, but it may
inhibit the progressive strength development because of its weak matrix
permitted ingress of carbonation[26,58]. The production of Calcite
crystals was increased under heat curing, and their appropriate amount
could be used as inert particles to fill the holes, thus improving the
Fig. 13. Differential distribution curves of pore structures. matrix compactness and mechanical properties [47].

4. Conclusions
Table 3
Volume ratios of pore structures.
The effects of various curing methods on the compressive strength
Curing Total Pore size distribution (%) and microstructure of SCBF were studied. The following conclusions can
method porosity
Mesopores Macropores Voids/ be deduced:
(%)
(3–50 nm) (50–10000 nm) microcracks (1) The early strength values obtained under normal temperature
(>10000 nm) curing (water and RT sealed) were quite low, reaching 4.4 and 6.1 MPa
Water 23.50 12.33 10.65 0.52 at 3d versus 20.4 and 22.6 MPa at 28d, respectively. The optimal heat
RT, sealed 21.35 11.59 9.30 0.46 curing scheme was 75 ◦ C at 12 h, providing the 3d/28d strength values
75 ◦ C@12 h 18.44 16.45 1.54 0.45
of 16.4/24.7 MPa. The latter values exceeded those of water curing and
90 ◦ C@12 h 32.41 19.21 12.05 1.15
75 ◦ C@24 h 38.35 19.72 16.76 1.87 RT sealed curing by 264/ 31 % and 154/24.5 %, respectively. The me­
chanical properties at early and later stages were significantly improved
under the optimal scheme.
reaction gel product generation is further promoted, more shrinkage (2) The hydration reaction under normal temperature curing devel­
cracks appear in the matrix, significantly increasing the number of large oped gradually. The optimal heat curing (75 ◦ C at 12 h) can effectively
pores and microcracks in the latter. Such initial defects deteriorate the accelerate the early hydration, increase the production of C–S–H gel,
late strength. HC, HT, and other crystals, significantly accelerating the consolidation

Fig. 14. Early microstructure development of SCBF under different curing methods.

10
W. Guo et al. Construction and Building Materials 357 (2022) 129397

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The authors declare that they have no known competing financial [20] W. Guo, Z. Zhang, Y. Bai, G. Zhao, Z. Sang, Q. Zhao, Development and
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