buildings

Article
Compressive Strength and Microstructure of Carbide Slag and
Alkali-Activated Blast Furnace Slag Pastes in China
Zhixin Li 1, *, Kaidong Xu 1, *, Nan Sun 2 , Jina Wang 1, *, Kaiwang Xue 1 , Longyun Xu 1 , Yi Ren 1 , Zhenzhou Yan 1
and Tongbao Sima 1

1 School of Material and Chemical Engineering, Henan University of Urban Construction,

Pingdingshan 467036, China; [email protected] (K.X.); [email protected] (L.X.);
[email protected] (Y.R.); [email protected] (Z.Y.); [email protected] (T.S.)
2 School of Civil and Transport Engineering, Henan University of Urban Construction,
Pingdingshan 467036, China; [email protected]
* Correspondence: [email protected] (Z.L.); [email protected] (K.X.); [email protected] (J.W.)

Abstract: The alkali-activated blast furnace slag is attracting significant attention in replacing Portland
cement due to several characteristics similar to cement hydration. However, there are a few practical
problems with commercial alkali activators, such as the fast setting time, relatively high costs, and
significant CO2 emissions during preparation. Thus, discovering industrial residues possessing
inherent alkalinity are urgent. This study proposes the use of carbide slag at levels of 0%, 5%, 10%,
15%, 20%, and 30% and alkali at levels of 1%, 2%, 3%, 4%, 5%, 6%, 8%, and 10% activated blast furnace
slag. The compressive strength and microstructure of carbide slag and alkali-activated blast furnace
slag (CAB) pastes were examined using X-ray diffraction analysis (XRD), Differential Scanning
Calorimetry/Thermogravimetric Analysis (DSC/TG), Fourier transform infrared spectroscopy (FTIR)
and Scanning electron microscopy (SEM). The results revealed that the addition of carbide slag
produced more hydrotalcite-like phase as well as decreased the content of ettringite (AFt) and the
calcium–silicate–hydrate (C-S-H) gel, which decreased the compressive strength of the CAB pastes.
At the age of 28 days, when the dosage was 5%, 10%, 15%, 20%, and 30%, the compressive strength
Citation: Li, Z.; Xu, K.; Sun, N.; Wang,
of CAB mixes decreased by 2.1%, 7.1%, 9.2%, 9.8%, and 28.1%, respectively. The addition of NaOH
J.; Xue, K.; Xu, L.; Ren, Y.; Yan, Z.; promoted the formation of AFt, and there was an optimum level of NaOH corresponding to the high
Sima, T. Compressive Strength and compressive strength of paste. At the age of 3 days and 7 days, the compressive strength reached its
Microstructure of Carbide Slag and maximum at the dosage of 6% NaOH, which was 24.8 MPa and 36.3 MPa, respectively. However, at
Alkali-Activated Blast Furnace Slag the ages of 14 days and 28 days, the compressive strength increased as the dosage of NaOH increased
Pastes in China. Buildings 2024, 14, to 5%, which was 43.3 MPa and 44.5 MPa, respectively. The water curing could both enhance the early
1681. https://doi.org/10.3390/ and later strength, the compressive strength of 23.3 MPa was gained at 3 days, and this increased by
buildings14061681 16.3%, 24.0% and 36.9% at 7 days, 14 days and 28 days, respectively. Therefore, water curing was
Academic Editors: Bjorn Birgisson suitable for the strength development of CAB pastes.
and Eugeniusz Koda
Keywords: compressive strength; microstructure; carbide slag and alkali activation; blast furnace slag
Received: 3 April 2024
Revised: 22 May 2024
Accepted: 30 May 2024
Published: 6 June 2024
1. Introduction
Increasing global CO2 has contributed to global warming and extreme weather
events [1]. Countries have reached a consensus on reducing CO2 emissions [2]. China is a
Copyright: © 2024 by the authors. major construction country and a major emitter of CO2 . As one of China’s pillar industries,
Licensee MDPI, Basel, Switzerland. the construction industry plays a crucial role in promoting China’s economic development.
This article is an open access article However, it also consumes a large amount of construction materials and emits massive
distributed under the terms and CO2 [3]. In 2020, the construction materials in China have emitted 1.48 billion tons of CO2 .
conditions of the Creative Commons
The cement industry is the largest carbon emitter in the construction materials industry,
Attribution (CC BY) license (https://
accounting for more than 80% of CO2 emissions [4]. With the accelerated development
creativecommons.org/licenses/by/
of urbanization in China, the total CO2 emissions from the Chinese cement industry will
4.0/).

Buildings 2024, 14, 1681. https://doi.org/10.3390/buildings14061681 https://www.mdpi.com/journal/buildings

Buildings 2024, 14, 1681 2 of 19

continue to increase if effective control measures are not taken. As a result, the prepa-
ration of low-carbon binders has been recognized as an effective measure to reduce the
carbon emissions from the Portland cement industry [5]. Many studies have focused on the
application of industrial waste by-products in construction materials [6–10].
In particular, the alkali-activated blast furnace slag is attracting significant attention
due to several characteristics similar to cement hydration. Huang et al. [11] studied the
kinetics of alkali–silica reaction-induced damage in alkali-activated granulated blast furnace
slag and showed that it depended on the alkali concentration and activator type. Li et al. [12]
discussed the effect of pH and temperature on the further slag hydration and demonstrated
that the low temperature and high pH of solution contributed to the further slag reaction.
Hruby et al. [13] carried out the resistance of alkali-activated blast furnace slag to acids and
indicated that it deteriorated when affected by acids. Usherov-Marshak et al. [14] studied
the hydration via calorimetric studies and thought that a high heat rate was a criterion
in the case of alkali-activated blast-furnace slag cements. Li et al. [15] used CaCl2 and
NaCl to improve the compressive strength of carbide slag-activated ground blast furnace
slag and found that the addition of CaCl2 and NaCl promoted the reaction of carbide slag,
and the contribution of CaCl2 was greater than NaCl. Lin et al. [16] investigated the soda
residue-activated blast furnace slag and considered that the addition of 2.5–10% CaCl2 was
beneficial for compressive strength improvement, and adding CaSO4 was harmful to the
compressive strength. Laurent et al. [17] studied the effect of CaCl2 on the blast furnace slag
hydration in blended cement and thought the CaCl2 improved the compressive strength
by 50%.
In addition, Karam et al. [18] found that sediment delayed the reaction at early age but
made a little contribution to the later age. Klimenko et al. [19] found interactions between
sodium silicate and sand depended on the degree of dispersibility. Bilici et al. [20] revealed
that the washing aggregate sludge waste reduced the compressive strength of alkali-
activated mortar samples. Occhicone et al. [21] showed the compressive strength of red
mud and blast furnace slag-activated materials up to 70 MPa. Niu et al. [22] incorporated
the bioleached sulfidic mine tailings into alkali-activated blast furnace slag and displayed
high compressive strength up to 90 MPa. Zhao et al. [23] revealed that the substitution ratio
of steel slag could not exceed 15%; otherwise, the mechanical properties would be reduced.
Feng et al. [24] reported that the addition of MgO and CaO improved the mechanical
strength of alkali-activated blast furnace slag. Huang et al. [25] found that the cations and
concentration have a great impact on the reaction process. Zhang et al. [26] showed that
the optimal Na2 O content of alkali-activated soda residue-blast furnace slag system was
3.0% considering the compressive strength. Despite the efforts of numerous researchers,
the application of alkali-activated blast furnace slag at construction sites is very limited due
to the existing commercial alkali.
Currently, the widely used commercial alkali activators are sodium hydroxide and
sodium silicates [27]. However, there are a few practical problems with commercial alkali
activators, such as fast setting time [28–32], relatively high costs [27,33] and significant
CO2 emissions [34–36] during preparation. Therefore, the search for cheap and low-carbon
activators that could replace commercial alkali has received a great deal of attention in
recent years.
Carbide slag is an industrial waste resulting from the hydrolysis of calcium car-
bide for the preparation of acetylene [27], and it is estimated that China produced about
5.6 × 107 tons of carbide slag per year [37]. However, carbide slag can only be used in
the production of cement with a utilization rate of less than 40% [38]. Most carbide slag
is stored in wet dam or dumps. This not only occupies a large amount of land but also
leads to the salinization of surrounding land and contamination of nearby surface and
groundwater sources [39]. Therefore, the recycling of carbide slag has attracted extensive
interest from many researchers.
Additionally, carbide slag is mainly composed of Ca(OH)2 , which is soluble in water
and strongly alkaline [38]. Thus, carbide slag has the potential to replace commercial
Buildings 2024, 14, 1681 3 of 19

alkali for the preparation of an alkali-activated binder. Furthermore, alkali-activated blast

furnace slag has the advantage of rapidly increasing strength even at room temperature [40].
Consequently, a carbide slag-activated blast furnace slag binder is prepared. Unfortunately,
the excitatory activity of Ca(OH)2 from carbide slag to blast furnace slag is very poor,
which still needs to be improved. Therefore, carbide slag blended commercial alkali as
the activator activating blast furnace slag to prepare low-carbon binder is studied. In
general, the principal hydration products with carbide slag and alkali-activated blast
furnace slag pastes are similar to those found with pure alkali activated blast furnace
slag pastes; however, the amount and timing of hydration products may be affected by
the added constituents. These changes would then be reflected in properties, such as
compressive strength. In order to understand and predict the performance of carbide slag
and alkali-activated blast furnace slag pastes, it is useful to study the compressive strength
and microstructure. The research results can provide a theoretical basis for the further
utilization of carbide slag and blast furnace slag.

2. Materials and Methods

2.1. Materials
The wet carbide slag used in this experiment was provided by Henan Shenma Chlor
Alkali Development Co., Ltd., Pingdingshan, China. The powered blast furnace slag
(S105) used in this study came from Gongyi Longze Water Purification Materials Co.,
Ltd. (Zhengzhou, China) with a bulk density of 488 kg/m3 . Their chemical composition,
mineralogical property and morphology were determined by X-ray fluorescence (XRF),
X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM). The chemical
composition of carbide slag was shown in Table 1, and its main component of CaO was
90.29%. Figure 1a showed the X-ray diffraction analysis of carbide slag, and the peaks at
2θ = 18.2◦ , 34.2◦ , and 47.2◦ were typical for Ca(OH)2 (CH). The morphology of carbide slag
is shown in Figure 2a. It displayed irregularity, and the particle size was approximately
between 5 and 45 µm through measurement. The chemical composition, X-ray diffraction
analysis and morphology of blast furnace slag are shown in Table 2, Figures 1b and 2b,
respectively. The main components of blast furnace slag were CaO, SiO2 and Al2 O3 . The
XRD analysis of blast furnace slag showed an obvious dispersion peak in the range of
25–35◦ , which indicated the presence of a large amount of amorphous peaks (glass phase).
The morphology of blast furnace slag presented irregular as well, and the particle size was
approximately between 2 and 25 µm. The hydraulic coefficient b, alkalinity coefficient
M0 , activity coefficient M1 and mass coefficient K of blast furnace slag were calculated via
Equations (1)–(4), which indicated blast furnace slag had high hydration activity. Sodium
hydroxide were analytical reagents and purchased from Yantai Shuangshuang Chemical
Co., Ltd., Yantai, China.

CaO + Al2 O3 + SiO2 42.21 + 15.62 + 27.24

b= = = 3.12 (1)
SiO2 27.24

WCaO + WMgO 42.21 + 9.01

M0 = = = 1.20 (2)
WSiO2 + WAl2 O3 27.24 + 15.62
WAl2 O3 15.62
M1 = = = 0.57 (3)
WSiO2 27.24
WCaO + WMgO + WAl2 O3 42.21 + 9.01 + 15.62
K= = = 2.31 (4)
WSiO2 + WMnO + WTiO2 27.24 + 0.47 + 1.22

Table 1. Chemical composition of carbide slag used (%).

Carbide Slag Na2 O MgO Al2 O3 SiO2 P2 O 5 SO3 Cl K2 O CaO TiO2 V2 O5 Fe2 O3 SrO
Chemical Composition 0.74 0.34 2.21 4.23 0.08 0.78 0.93 0.01 90.29 0.05 0.02 0.24 0.08
Buildings
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19
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40 Amorphous peak
(glass phase)
40 Amorphous peak
35
(glass phase)
35
30
30

Intensity (Counts/s)
25

Intensity (Counts/s)
25
20
20
15
15
10
10
5
5
0
0
-5
0 10 20 30 40 50 60 70
-5
0 2θ(degree)
10 20 30 40 50 60 70

(a) (b) 2θ(degree)

(a) (b)
Figure
Figure 1.
1. (a,b)
(a,b) XRD
XRD pattern
pattern of
of carbide
carbide slag
slag and
and blast
blast furnace
furnace slag.
slag.
Figure 1. (a,b) XRD pattern of carbide slag and blast furnace slag.

(a) (b)
(a) (b)
Figure 2. Morphology of carbide slag and blast furnace slag: (a) carbide slag and (b) blast furnace
Figureof2.carbide
Figure 2. Morphology
slag. Morphology of blast
slag and carbide slag and
furnace slag:blast furnace
(a) carbide slag:
slag and (a)(b)
carbide slag and
blast furnace (b) blast fur
slag.
slag.
Table 1.
Table Chemical composition of carbide
2. Chemical blast furnace slag (%).
slag used used (%).
Table 1. Chemical composition of carbide slag used (%).
Carbide
Blast Slag
Furnace Slag Na22OO MgO
Na MgOAl2 Al O3 2 SiO
O3 2SiO SO23 P2O Cl5 SO K23O ClCaOK2O TiOCaO2 MnO TiOFe22 OV O5 FeY22O
3 2SrO O33 SrO
ZrO2
Chemical Carbide Slag
Composition Na
0.74 9.010.3415.62 2O
2.21 MgO Al 2O3 SiO2 P2O5 SO3 Cl K2O 0.02CaO TiO2 V 2O5 Fe2O3
Chemical Composition 0.48 27.24 4.23
2.73 0.08
0.07 0.78
0.42 0.93 0.011.2290.29
42.21 0.47 0.05
0.40 0.07 0.24
0.01 0.08
0.06
Chemical Composition 0.74 0.34 2.21 4.23 0.08 0.78 0.93 0.01 90.29 0.05 0.02 0.24
Table 2. Chemical composition of blast furnace slag used (%).
2.2. Mixture Proportions
Table 2. Chemical composition of blast furnace slag used (%).
Blast Furnace Slag Na2O MgOof Al
Details 2O3 SiO2 SO3 Cl K2O CaO TiO2 MnO Fe2O3 SrO Y2O3 ZrO2
carbide slag and alkali-activated blast furnace slag paste (CAB) mixtures
Blast Furnace
Chemical Composition Slag9.01 Na 2O MgO Al2O3 SiO2 SO3 Cl K2O CaO TiO2 MnO Fe2O3 SrO Y2O3
tested in this study are27.24
0.48 15.62 2.73 0.07
presented 0.42 3–5.
in Tables 42.21
In all1.22
CAB0.47 0.40the0.07
mixtures, 0.01
spread flow0.06
was
Chemical Composition 0.48 9.01 15.62 27.24 2.73 0.07 0.42 42.21 1.22 0.47 0.40 0.07 0.01
kept constant at (120 ± 5) mm. The carbide slag for each CAB mixture was dried in an
electric oven and ground in a laboratory steel ball mill. The alkaline activator for each CAB
mixture was prepared CaO + Al2O3 +anSiO 42.21 + 15.62 + 27.24
b =by dissolving alkaline compound
CaO=+ Al2O3 + SiO2 42.21=
2 into tap water before mixing.
3.12
+ 15.62 + 27.24 (1)
The effects of the carbide slag toSiO 2b =furnace slag paste
blast 27.24ratio,
= alkali activator, and = 3.12
curing
conditions were investigated by varying design SiO
factors.
2 27.24
M1, M7 and M15 were designed as the reference CAB paste. The interaction between
carbide slag and blast furnace slagW in +CAB
WMgOpastes was+studied
42.21 9.01 by using different combina-
M = CaO = WCaO + WMgO = 1.20 42.21 + 9.01 (2)
tions of carbide slag and blast0 furnace
WSiO2 + WAlM2O03 = 27.24 +15.62
slag in M1 to M6. = M14 were designed
M7 to = 1.20 to study
the effect of elevating sodium hydroxide activator 2
+ WAl2O3 and27.24
WSiO(NaOH), M15+to15.62
M17 were designed
to study the effect of curing conditions. The standard curing was at 20 ◦ C and 95% relative
humidity, the sample was put into water for curing. The steam curing was autoclaved at
120 ◦ C for 8 h and then cured under standard conditions.
Buildings 2024, 14, 1681 5 of 19

Table 3. Mixture proportion of CAB pastes (carbide slag to blast furnace slag ratio).

Blast Furnace Sodium Curing

Mix Carbide Slag
Slag Hydroxide Conditions
M1 100% 0% 3% Standard curing
M2 95% 5% 3% Standard curing
M3 90% 10% 3% Standard curing
M4 85% 15% 3% Standard curing
M5 80% 20% 3% Standard curing
M6 70% 30% 3% Standard curing

Table 4. Mixture proportion of CAB pastes (NaOH).

Blast Furnace Sodium Curing

Mix Carbide Slag
Slag Hydroxide Conditions
M7 80% 20% 1% Standard curing
M8 80% 20% 2% Standard curing
M9 80% 20% 3% Standard curing
M10 80% 20% 4% Standard curing
M11 80% 20% 5% Standard curing
M12 80% 20% 6% Standard curing
M13 80% 20% 8% Standard curing
M14 80% 20% 10% Standard curing

Table 5. Mixture proportion of CAB pastes (curing conditions).

Blast Furnace Sodium Curing

Mix Carbide Slag
Slag Hydroxide Conditions
M15 90% 10% 3% Standard curing
M16 90% 10% 3% Water curing
M17 90% 10% 3% Steam curing

2.3. Experimental Method (Sample Preparation) (Figure 3)

(1) Water-to-Solid Ratio Test
The water-to-solid ratio of the CAB pastes was measured using a slump test according
to GB/T 8077-2012 <Methods for testing uniformity of concrete admixture> [41]. The test
procedure as follows: the glass plate, truncated cone round mold, agitator and stirring pot
were wiped to make their surfaces wet without water stains. The glass plate was put in
a horizontal position, and the truncated cone round mold (height 60 mm, top diameter
36 mm and bottom diameter 60 mm) was placed in the center of the glass plate. Then, 300 g
of CAB mixture was weighed and added to the mixing water, which dissolved alkaline.
This was followed by stirring for 4 min. Next, the paste was transferred into a truncated
cone round mold placed on a glass plate and then vertically lifted. The resulting spread of
paste was measured twice, the second measurement being perpendicular to the first. The
final spread flow value was taken as the average of the two value measured. At last, the
final water to solid ratio yielding a spread flow of (120 ± 5) mm was achieved.
(2) Determination of Setting Time
The setting time was tested according to GB/T 1346-2011 <Test method for water
requirement of normal consistency, setting time and soundness of the Portland cement> [42].
Briefly, 500 g of CAB mixture was slowly added to the measured water, which dissolved
alkaline. The suspension was mixed for 4 min to form a homogenous paste, and then the
paste was cast into pieces (height 40 mm, top diameter 65 mm and bottom diameter 75 mm).
The entrained air was removed by tapping the slurry beyond the test mold 5 times using a
right angle knife. Excess paste was sawed off gently at about 1/3 of the upper surface of
Buildings 2024, 14, 1681 6 of 19

the test mold. When the test needle sank to (4 ± 1) mm from the bottom plate, the paste
reached the initial setting state. When the test needle sank 0.5 mm into the test body, the
paste reached the final setting state.
(3) Compressive Strength
The compressive strength was measured according to GB/T 17671-2021 <Test method of
cement mortar strength (ISO method)> [43]. Six replicate specimens (40 mm × 40 mm × 80 mm)
were prepared for each condition (time and dosage) to obtain the average and variability in
compressive strength test results. Briefly, 1 kg of CAB mixture was slowly added to the
measured water. The suspension was mixed for 4 min to form a homogenous paste, and
then the pastes were filled into molds. The entrained air was removed by lifting the mold
by approximately 1 cm and subsequent dropped. This procedure was repeated 5 times.
Excess paste was removed by scratching the surface with a ruler. After 1 days, the molds
Buildings 2024, 14, x FOR PEER REVIEW 7 of 21
was dismantled, compressive strength was measured after 3 days, 7 days, 14 days and
28 days.

(a) (b) (c)

Figure 3.
Figure 3. Photos
Photosduring
duringtesting
testingofofwater
watertoto
solid ratio,
solid setting
ratio, time,
setting andand
time, compressive strength:
compressive (a)
strength:
water to solid ratio; (b) setting time; (c) compressive strength.
(a) water to solid ratio; (b) setting time; (c) compressive strength.

2.4. Materials
2.4. Materials Characterization
Characterization
After the
After the testtestspecimens
specimens were
were cured
cured for corresponding
for the the corresponding time under
time under specified
specified condi-
conditions,
tions, hydrationhydration was terminated
was terminated with absolute
with absolute ethanol, ethanol, and the specimens
and the specimens were driedwere
in a
dried in drying
vacuum a vacuum ovendrying
at 45 ◦oven
C for at
24 45 °C for 24by
h, followed h, XRD,
followed by XRD,
DSC/TG, FTIRDSC/TG,
and SEMFTIR and
analysis.
SEMAfter
analysis.
the hydration of CAB pastes, CAB paste samples of various ages were ground
After the hydration
into fine powder of CAB
for analysis. Thepastes,
resultingCAB paste product
reaction samplesassemblage
of various ages were ground
was characterized
into fine powder for analysis. The resulting reaction product
by XRD. The measurements were made using a X’ Pert pro diffractometer equipped with assemblage wasa
characterized
CoKα X-ray tube by operated
XRD. Theatmeasurements
40 kV voltage and were40mademA with using a X’
step of Pert ◦
0.02 pro
(2θ)diffractometer
and scanning
equipped
time s/◦ . The
of 30 with a CoKα
CABX-ray
pastetube operated
samples wereat 40 kV voltage
scanned between 5◦ 40
and andmA65◦with
(2θ).step of 0.02°
(2θ) The
and characteristic
scanning timefunctional
of 30 s/°. groups
The CAB paste
of the samples
phases were
present in scanned
CAB paste between
samples5°were
and
65° (2θ).using a ThermoFisher Nicolet FT-IR spectrometer. The background spectrum was
studied
The characteristic
collected using a pure KBr functional groups
pellet, and the of the phases
infrared Fourier present in CAB
transform paste samples
spectroscopy were
enabled
studied using of
measurement a ThermoFisher Nicolet
the range between FT-IR
4000 andspectrometer.
400 cm . − 1 The background spectrum was
collected using a puredifferential
A simultaneous KBr pellet, and the infrared
scanning Fourier transform spectroscopy
calorimetry/thermogravimetric enabled
analysis was
measurement
carried out byof the range
Netzsch STAbetween
449 F3 4000 andunder
Jupiter 400 cm −1.
nitrogen atmosphere. Approximately
10 mgAofsimultaneous
the samples was differential scanning
heated from temperature to 1000 ◦ C with a heating
room calorimetry/thermogravimetric analysis was
rate of
10 ◦ C/min
carried out in byan Al2 O3 STA
Netzsch crucible
449 with an identical
F3 Jupiter crucible as
under nitrogen reference. Approximately 10
atmosphere.
mg ofThethemorphological
samples was heatedinvestigations
from room of hydration
temperature products
to 1000were observed
°C with a heatingby rate
scanning
of 10
electron
°C/min in microscopy (QUANTA
an Al2O3 crucible with450). The pieces
an identical were coated
crucible with a Au-Pd layer to improve
as reference.
conductivity and image quality
The morphological before the
investigations test.
of hydration products were observed by scanning
electron microscopy (QUANTA 450). The pieces were coated with a Au-Pd layer to
improve conductivity and image quality before the test.
 2024, 14,
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2.5. Experimental Techniques

2.5. Experimental Techniques
Figure
Figure 44 exhibits
exhibits the
the process
process flow
flow diagram.
diagram.

Figure 4.
Figure 4. The
The process flow diagram.
process flow diagram.

3. Results and
3. Results and Discussion
Discussion
3.1. Properties
3.1. Properties
3.1.1. Effect of Carbide Slag to Blast Furnace Slag Ratio on Properties of CAB Pastes
3.1.1. Effect of Carbide Slag to Blast Furnace Slag Ratio on Properties of CAB Pastes
The water-to-solid ratio, setting time and compressive strength of the CAB pastes
The water-to-solid ratio, setting time and compressive strength of the CAB pastes
were measured (Figure 5). Figure 5a showed the water-to-solid ratio increased slightly
were measured (Figure 5). Figure 5a showed the water-to-solid ratio increased slightly
with a different carbide slag to blast furnace slag ratio when the slump flow of CAB pastes
withfixed
was a different
at (120carbide
± 5) mm slagbytoadjusting
blast furnace slag ratio
the water whenInthe
content. slump
Figure 5b,flow
it can of be
CAB pastes
seen that
was fixed at (120 ± 5) mm by adjusting the water content. In
there was a small increase trend in the setting time for CAB pastes. At the carbide slagFigure 5b, it can be seen that
to
therefurnace
blast was a small increase
slag ratio trendthe
of 0:100, in initial
the setting
settingtime
timeforwas
CAB 63 pastes.
min, and Atitsthefinal
carbide
was 31slag to
min
blast furnace slag ratio of 0:100, the initial setting time was 63 min,
longer than the initial. The initial and final setting times increased steadily to 75 min and and its final was 31 min
longer
105 minthan
when thetheinitial.
carbide Theslag
initial and final
to blast furnacesetting
slag times increased
ratio was 30: 70.steadily
This cantobe75due mintoand
the
decrease of blast furnace slag, and the excitation effect of carbide slag was far weakertothan
105 min when the carbide slag to blast furnace slag ratio was 30: 70. This can be due the
decrease of blast
that of sodium hydroxide.furnace slag, and the excitation effect of carbide slag was far weaker than
that of sodium hydroxide.
Measurements of compressive strength hydrated for 3 days, 7 days, 14 days and
Measurements
28 days were shown in Figure of compressive strength
5c. Clearly, hydrated for
the compressive 3 days,of7 CAB
strength days,pastes14 days and 28
decreased
days were shown in Figure 5c. Clearly, the compressive strength
with increasing carbide slag substitution ratio and increased with longer curing time. At of CAB pastes decreased
3with
days,increasing carbide strength
the compressive slag substitution
of the M1,ratioM2,andM3,increased
M4, M5, and with M6longer
mixescuringwas 19.8time.
MPa,At
3 days, the compressive strength of the M1, M2, M3, M4, M5,
19.5 MPa, 19.0 MPa, 17.9 MPa, 16.5 MPa, and 15.5 MPa, respectively. After 7 days, the and M6 mixes was 19.8 MPa,
19.5 MPa, 19.0
compressive MPa, 17.9
strength of theMPa,M1,16.5M2,MPa,M3, and
M4, 15.5
M5, MPa,
and M6 respectively.
mixes improvedAfter 7 by days, the
39.9%,
compressive
40.5%, 41.6%,strength
44.1%, 31.5%,of the andM1,6.5%,
M2, M3, M4, M5, At
respectively. and14M6 mixes
days, the improved
improvement by 39.9%,
in the
40.5%, 41.6%,strengths
compressive 44.1%, 31.5%, and M2,
of the M1, 6.5%, M3,respectively.
M4, M5, and AtM614 mixes
days, was
the improvement
58.6%, 58.5%, 60.5%, in the
compressive strengths of the M1, M2, M3, M4, M5, and M6 mixes
67.6%, 66.7%, and 33.5%, respectively. After 28 days curing, the M1, M2, M3, M4, M5, and was 58.6%, 58.5%, 60.5%,
67.6%,
M6 66.7%,
mixes and 33.5%, the
outperformed respectively.
3-day mixAfter 28 days
by 70.7%, curing,
69.7%, the M1,
65.3%, M2,84.9%,
71.5%, M3, M4, and M5, and
56.8%,
M6 mixes outperformed
respectively. It was noteworthy the 3-day thatmixtheby 70.7%, 69.7%,
compressive 65.3%,of71.5%,
strength M1–M6 84.9%, and 56.8%,
decreased with
respectively.
increasing It wasslag
carbide noteworthy
substitutionthat ratio
the compressive
at the same strength
curing time. of M1–M6
Note that decreased with
the greatest
increasing carbide
compressive strength slag substitution
appeared in theratio
CABat the same
pastes curing
with the time.
lowest Note slag
carbide that content.
the greatest
The
highest
compressivecompressive
strengthstrength
appeared (1–28
in the days)
CABoccurred in M1,
pastes with theand its compressive
lowest carbide slag strength
content.
was
The 19.8 MPacompressive
highest at 3 days, 27.7strengthMPa at 7(1–28 days,days)
31.4 MPa at 14 days,
occurred in M1,andand 33.8its MPa at 28 days.
compressive
At the curing
strength was 19.8timeMPa of 3atdays,
3 days,the27.7
M2,MPa M3,atM4, M5, 31.4
7 days, and MPaM6 mixes underperformed
at 14 days, and 33.8 MPathe at
control
28 days.mix by curing
At the 1.5%, 4.0%,
time of 9.6%, 16.7%,
3 days, and M3,
the M2, 21.7%,
M4,respectively.
M5, and M6 mixes At 7 days, the M2, M3,
underperformed
M4, M5, and
the control mixM6by mixes
1.5%,exhibited
4.0%, 9.6%, a lag of 1.1%,
16.7%, and2.9%,
21.7%, 6.9%, 21.7%, and
respectively. At40.43%,
7 days, respectively,
the M2, M3,
compared
M4, M5, and to M6
the control mix. At 14
mixes exhibited days,
a lag the compressive
of 1.1%, 2.9%, 6.9%,strength
21.7%, and of M2,
40.43%,M3, respectively,
M4, M5, and
M6 mixes showed
compared a lag ofmix.
to the control 1.6%,At2.9%, 4.5%,the
14 days, 12.4%, and 31.4%,
compressive respectively,
strength of M2, compared
M3, M4,with M5,
the control mix. After 28 days, the compressive strength of M2,
and M6 mixes showed a lag of 1.6%, 2.9%, 4.5%, 12.4%, and 31.4%, respectively, compared M3, M4, M5, and M6 mixes
decreased by 2.1%,
with the control mix. 7.1%,
After9.2%, 9.8%,the
28 days, and 28.1%, respectively.
compressive strength of Therefore,
M2, M3, M4, the compressive
M5, and M6
Buildings 2024, 14, x FOR PEER REVIEW 9 of 21

Buildings 2024, 14, 1681 8 of 19

mixes decreased by 2.1%, 7.1%, 9.2%, 9.8%, and 28.1%, respectively. Therefore, the
compressive strength
strength of CAB pastes of CAB pastes
decreased with decreased
the increasewith the increase
of carbide of observation
slag. This carbide slag.was
This
in
observation wasthe
agreement with in agreement with
discovery of Seothe discovery
et al. [39], whoofdeemed
Seo et al. [39],
that thewho deemed strength
compressive that the
compressive strength
of the mixtures of slag
of carbide the mixtures of carbide
and blast furnace slagslag and diminished
linearly blast furnace slag
as the linearly
amount of
diminished
carbide slagas the amount of carbide slag increased.
increased.
130
(a) (b)
0.56
120
Initial
110
Final
0.52
100
Water to solid ratio

Setting time(min)
90
0.48
80

70
0.44
60

50
0.40
0:100 5:95 10:90 15:85 20:80 30:70
0:100 5:95 10:90 15:85 20:80 30:70
Carbide slag to blast furnace slag ratio
Carbide slag to blast furnace slag ratio
40
3-days (c)
7-days
35 14-days
28-days
30
Strength (MPa)

25

20

15

10
0:100 5:95 10:90 15:85 20:80 30:70
Carbide slag to blast furnace slag ratio

Figure
Figure 5.
5. (a–c)
(a–c) Effect
Effect of
of carbide
carbide slag
slag to
to blast
blast furnace
furnace slag
slag ratio
ratio on
on properties of CAB
properties of CAB pastes.
pastes.

3.1.2. Effect
Effect of
of NaOH
NaOH on Properties of CAB Pastes
The water-to-solid
water-to-solidratio, ratio,setting
settingtime
time and
and compressive
compressive strength
strength of CAB
of the the CABpastes pastes
with
increasing
with NaOH
increasing were were
NaOH measured (Figure
measured 6). Figure
(Figure 6a shows
6). Figure that the
6a shows thatwater-to-solid
the water-to-solid ratio
decreased
ratio slightly
decreased as theas
slightly dosage of NaOH
the dosage increased.
of NaOH It decreased
increased. to 0.49 to
It decreased at 0.49
the dosage
at the
of 4% and
dosage of 4%then
andfurther decreased
then further to 0.45toat0.45
decreased theatdosage of 10%.
the dosage In Figure
of 10%. In Figure6b, 6b,
it could be
it could
observed
be observedthatthat
there waswas
there an decreasing
an decreasing trendtrend
in theinsetting time for
the setting time CAB
for pastes. The initial
CAB pastes. The
and final
initial andsetting time of
final setting timeM7ofwasM7 89
wasmin and and
89 min 119 119
min,min,andandit decreased
it decreased dramatically
dramatically to
53 min and 89 min at the dosage of 5%. At last,
to 53 min and 89 min at the dosage of 5%. At last, it decreased againit decreased again but more steeply to
27 min and 68 min.
The compressive
The compressive strengthstrength development
development ofofCAB CABpastespastesafter
afteradding
adding NaOHNaOH waswasre-
ported in in
reported Figure
Figure 6c.6c.
TheTheinfluence
influenceof NaOH
of NaOH on the on strength
the strengthof CAB pastespastes
of CAB showed a trend
showed a
of increasing first and then decreasing, and the effects of different
trend of increasing first and then decreasing, and the effects of different NaOH content on NaOH content on the
strength
the results
strength were were
results close to eachtoother
close eachfromother 3 days
fromto328 days.
days toThe compressive
28 days. strength of
The compressive
strength of M12 after 3 days and 7 days of curing tended to level off (24.8 MPacompared
M12 after 3 days and 7 days of curing tended to level off (24.8 MPa and 36.3 MPa) and 36.3
to thecompared
MPa) others, and to the
the compressive
others, and the strength of M11strength
compressive after 14 of daysM11 and 28 14
after days
days of and
curing
28
tended to level off (43.3 MPa and 44.5 MPa) relative to the others.
days of curing tended to level off (43.3 MPa and 44.5 MPa) relative to the others. The The highest compressive
strengthcompressive
highest at 3 days and 7 days at
strength was achieved
3 days and 7for M12,
days wasindicating
achievedthat for the
M12,optimum
indicating NaOHthat
content was 6 wt% in terms of strength performance at 3 days
the optimum NaOH content was 6 wt% in terms of strength performance at 3 days and and 7 days. In addition, the
7
highest compressive strength at 14 days and 28 days was achieved
days. In addition, the highest compressive strength at 14 days and 28 days was achieved for M11, indicating that
the M11,
for optimum NaOHthat
indicating content was 5 wt%
the optimum NaOHin terms of the
content wasstrength
5 wt% in performance
terms of theatstrength
14 days
and 28 days.
performance at 14 days and 28 days.
 x FOR PEER REVIEW
Buildings 2024, 14, 1681 109of
of 21
19

0.7 160
(a) (b)
140
Initial
0.6 120 Final

100

Setting time (min)

Water solid ratio

80
0.5

60

40
0.4
20

0
0.3
0 2 4 6 8 10 0 2 4 6 8 10

Dosages (%) Dosages (%)

3-days (c)
60
7-days
14-days
50 28-days

40
Strength (MPa)

30

20

10

0
1% 2% 3% 4% 5% 6% 8% 10%
Dosages (%)

Figure 6. (a–c)
Figure 6. (a–c) Effect
Effect of
of NaOH
NaOH on
on properties of CAB
properties of CAB pastes.
pastes.

Effect of Curing Conditions on Properties of CAB Pastes

3.1.3. Effect
The compressive strength of the CAB pastes under different different curing conditions was
measured in Figure 7. Clearly, the compressive strength can be observed to increase with
time under standard curing curing condition
condition and and water
water curing
curing condition.
condition. At standard curing
condition, the compressive
compressive strength
strength of of 19.0
19.0 MPa was obtained at 3 days, and this increased increased
by 51.6%, 60.5% and 65.3% at 7 days, 14 days and 28 days, respectively.
days and 28 days, respectively. At At water curing
condition, the compressive strength of 23.3 MPa was gained at 3 days, and this increased
by 16.3%,
by 24.0%, and
16.3%, 24.0%, and 36.9%
36.9% at at 77 days,
days, 14
14 days
days and
and 28 28 days,
days, respectively.
respectively. However,
However, the the
compressive strength
compressive strength ofof 25.8
25.8 MPa
MPa waswas gained
gained atat 33 days,
days, and
and this
this increased
increased by by 7.0%
7.0% andand
15.1%
15.1% as
as the
the time
time increased
increased from
from 77 days
days toto 14
14 days
days whenwhen curing
curing atat steam
steam condition.
condition. The The
curing time in the excess of 14 days resulted in the negative trend in
curing time in the excess of 14 days resulted in the negative trend in terms of strength terms of strength
development. In
development. In addition,
addition,thethecompressive
compressivestrengths
strengthsofof25.825.8MPa
MPaatat3 days
3 days and
and 27.6
27.6MPaMPaat
7 days of M17 were observed, which were higher than M15 and M16
at 7 days of M17 were observed, which were higher than M15 and M16 at the same curing at the same curing
time. This
time. This value
value was
was close
close toto the
the compressive
compressive strength
strength at at 14
14 days
days under
under thethe standard
standard
curing condition and water curing condition, and it decreased to 28.2 MPa at 28
curing condition and water curing condition, and it decreased to 28.2 MPa at 28 days. This
days. This
indicated that the steam curing condition enhanced early strength
indicated that the steam curing condition enhanced early strength development, and development, and it wasit
not conductive
was to the to
not conductive later
thestrength development.
later strength Furthermore,
development. the compressive
Furthermore, strengths
the compressive
of 23.3 MPa
strengths at 3 MPa
of 23.3 daysatand 27.1and
3 days MPa at MPa
27.1 7 daysat 7ofdays
M16ofwere
M16observed to be higher
were observed than
to be higher
M15, and this number was close to each other at after 14 days and 28 days of curing time.
than M15, and this number was close to each other at after 14 days and 28 days of curing
This meant that the water curing condition enhanced early strength development as well
time. This meant that the water curing condition enhanced early strength development as
and contributed to the later strength. Thus, it could be concluded that the water curing
well and contributed to the later strength. Thus, it could be concluded that the water
condition was suitable for the development of compressive strength. Compared with the
curing condition was suitable for the development of compressive strength. Compared
previous similar study on fly ash geopolymer activated by carbide slag, the compressive
with the previous similar study on fly ash geopolymer activated by carbide slag, the
strengths of CAB pastes were significantly high at 3 days, 7 days and 28 days [44].
compressive strengths of CAB pastes were significantly high at 3 days, 7 days and 28 days
[44].
Buildings2024,
Buildings 2024,14,
14,1681
x FOR PEER REVIEW 11 of 21
10 of 19

45
3-days
40 7-days
14-days
35
28-days
30

Strength (MPa)
25

20

15

10

0
Standard curing Water curing Steam curing

Figure 7.
Figure 7. Effect
Effect of
of curing
curing conditions
conditions on
on compressive
compressive strength
strengthof
ofCAB
CABpastes.
pastes.

3.2.
3.2. Reaction
Reaction Products
Products
3.2.1. XRD Findings
3.2.1. XRD Findings
Based on the study of Li et al. [15], after adding blast furnace slag and carbide slag
Based on the study of Li et al. [15], after adding blast furnace slag and carbide slag
into water, the blast furnace slag released Ca2+ ,2+and the Ca2+ 2+and OH−- of carbide slag was
into water, the blast furnace slag released Ca , and the Ca and OH of carbide slag was
substantially dissolved into solution. The increased alkalinity in the solution disrupted
substantially dissolved into solution. The increased alkalinity in the solution disrupted Si-
Si-O-Si, Si-O-Al and other bonds, and it promoted the reaction of the decomposed glass
O-Si, Si-O-Al and other bonds, and it promoted the reaction of the decomposed glass
phase into hydration products. When the NaOH was added into the solution, the increased
phase into hydration products. When the NaOH was added into the solution, the
content of OH− in the solution increased the alkalinity and accelerated the reaction of
increased content of OH- in the solution increased the alkalinity and accelerated the
carbide slag and blast furnace slag.
reaction
The of carbide
results of slag and blast
the XRD furnace
analysis slag.
of hardened paste samples with different carbide
slag to The results
blast of theslag
furnace XRDratios
analysis of hardened
obtained at the paste
curing samples
stages with
of 28different
days are carbide
shownslag in
to blast furnace slag ratios obtained at the curing stages
Figure 8. In all samples, the main reaction products were calcium silicate hydrate of 28 days are shown in Figuregel 8.
In all samples, the main reaction products were calcium silicate
(C-S-H, PDF# 00-33-0306), monosulfoaluminate (AFm, PDF# 01-083-1289), ettringite (AFt, hydrate gel (C-S-H, PDF#
00-33-0306),
PDF# monosulfoaluminate
00-041-1451), and hydrotalcite-like (AFm, PDF# phase01-083-1289), ettringite (AFt,
(Ht, PDF# 00-014-0191). PDF#carbide
Adding 00-041-
1451),
slag and hydrotalcite-like
produced calcium hydroxide phase(CH, (Ht,PDF#
PDF#01-081-2040)
00-014-0191). and Adding
calcitecarbide
(C, PDF# slag produced
01-086-2340).
These were the same as the hydration products discovered by Seo et al. using XRDwere
calcium hydroxide (CH, PDF# 01-081-2040) and calcite (C, PDF# 01-086-2340). These [39].
the same as
However, nothe hydration
calcium products
hydroxide discovered
and calcite by SeoinetM1.
was found al. using XRD peak
The profile [39]. However,
intensities no of
calcium were
samples hydroxide
compared and tocalcite
assesswas found in M1.
approximately theThe profile
relative peak intensities
quantities of reaction ofproducts.
samples
were
To ourcompared
surprise, the to assess
C-S-Happroximately
gel located at ~29 the◦relative
and ~32quantities of reaction
◦ (2θ) decreased withproducts.
the increase To
our
of surprise,
carbide the
slag, andC-S-H gel located
the peaks of calciteat ~29°
and andC-S-H~32°gel(2θ)
were decreased with the
both detected at ~29increase
◦ . Thus,of
itcarbide
could slag, and thethat
be deduced peakstheofaddition
calcite and C-S-H gel
of carbide slagwere both the
reduced detected
contentat of
~29°.C-S-HThus, it
gel.
could
The be deduced
formation of AFtthatandthe AFm
addition
is made of carbide
possibleslag reduced
through the
the content of
presence of soluble
C-S-H gel. The
sulfate
formationwithin
(gypsum) of AFttheand AFm
blast furnaceis made
slag. The possible through
intensity of thetheAFtpresence
phase was ofalso
soluble sulfate
diminished
(gypsum) within the blast furnace slag. The intensity of
in the M3 and M5 mixture. This phenomenon was also found by Seo [39], who thought the AFt phase was also diminished
in the
the M3 and
intensity of M5
AFt mixture.
decreasedThis phenomenon
as the was alsoslag
amount of carbide found by Seo The
increased. [39],C-S-H
who thought
gel and
the intensity
AFt are the mainof AFt decreased
source as thedevelopment
of strength amount of carbide slag increased.
for samples. However, The C-S-H
note thatgel and
strong
AFt are
AFm the were
peaks mainproduced
source of in strength
the XRD development
pattern of M3 for and
samples. However,
M5, which showednotethatthatcarbide
strong
AFmpromoted
slag peaks were theproduced
formationinofthe AFmXRD andpattern of M3 andthe
thus inhibited M5, which showed
formation of AFt,thatwhich carbide
was
slag promoted
indicative of the thelowformation
strengthofofAFm M3 and and thus
M5. inhibited
Furthermore, the formation
there wasofaAFt,slightwhich
peakwas at
11.6 ◦ (2θ) in M1, indicating a hydrotalcite-like phase. This phase has been detected more
indicative of the low strength of M3 and M5. Furthermore, there was a slight peak at 11.6°
obviously
(2θ) in M1, in mixtures
indicating with the addition of carbide
a hydrotalcite-like phase.slag.ThisThis situation
phase was consistent
has been detected more with
the findingsinofmixtures
obviously Seo [39],with whothe considered
addition that the peak
of carbide intensity
slag. of carbide
This situation wasslag increased
consistent as
with
the
the carbide
findingsslagof Seocontent
[39], increased.
who considered It indicated
that the that
peakcarbide slag of
intensity promoted the formation
carbide slag increased
of
as the carbide
hydrotalcite-like
slag content phase. Concerning
increased. the reaction
It indicated that carbidedegreeslagof carbide slag,
promoted calcium
the formation
hydroxide
of the hydrotalcite-like phase. Concerning the reaction degree of carbide slag, calcium
and calcite were identified for M3 and M5, and the intensity of the calcium
hydroxide
hydroxide and and calcite
calcite increased
were identifiedwith the for increase
M3 and of M5,carbide
and the slag. This meant
intensity of the that the
calcium
carbide slag was not fully involved in the reaction. These
hydroxide and calcite increased with the increase of carbide slag. This meant that theresults match well with those of
the mechanical
carbide slag was strength.
not fullyThus,
involvedthe compressive
in the reaction. strength
Theseofresults
M3 and M5 decreased.
match well with those of
the mechanical strength. Thus, the compressive strength of M3 and M5 decreased.
Buildings 2024, 14, x FOR PEER REVIEW 12 of 21

Buildings 2024,
Buildings 14, 14,
2024, 1681x FOR PEER REVIEW 12 of 21 11 of 19

Ht S
140
AFt AFt AFt C S
Ht S
140
120 AFt AFt CH AFt C S CH
CH CH 1.5%
120
100 1.5%
100
80
80

60 0.5%
60 0.5%

40
40

20
20 0% 0%

00
0 10
10 2020 30 30 40 40 50 50 60 60 70 70
2θ(°2θ(
) °)
Figure 8.
Figure 8. XRD
XRDanalyses
analyses ofof
pastes with
pastes different
with carbide
different
different slag toslag
carbide blast
tofurnace slag ratios
blast furnace at ratios
slag the curing
at the curing
age of 28 days. Ht: hydrotalcite-like phase, CH: calcium hydroxide, S: C-(A)-S-H gel, C: calcium
age of 28
28 days.
days. Ht: hydrotalcite-like
hydrotalcite-like phase, CH: calcium hydroxide, S: C-(A)-S-H gel, C: calcium
carbonate, AFt: ettringite.
carbonate, AFt: ettringite.
carbonate, AFt: ettringite.
The XRD patterns of hardened paste samples with different NaOH dosages obtained
at theThe XRD
curing patterns
stages of 28 of hardened
days are shown paste samples
in Figure with different
9. Similar different NaOH
to the different dosages
carbide slagobtained
at
tothe curing
curing
blast furnacestages
stages of28
of
slag ratio 28 daysare
days
mixtures, are shown
C-S-Hinin
shown
the Figure
Figure
gel, 9.9.Similar
AFt, AFm, Similartoto the
the different
different
and hydrotalcite-like carbide
carbide
phases slag
slag to
to blast
blast
were thefurnace
furnace
main slagslag ratio
ratio
reaction mixtures,
mixtures,
phases observed the
the C-S-H
C-S-H
with gel,AFt,
gel, AFt,and
all mixtures, AFm,
AFm, andhydrotalcite-like
theand hydrotalcite-like
characteristic peaks of phases
were thehydroxide
calcium main reaction phases
and calcite stillobserved with
existed. The all mixtures,
diffraction and
patterns of the characteristic
calcium hydroxide,peaks of
calcite and
calcium C-S-H geland
hydroxide showed only
calcite stillsome differences
existed. in intensitypatterns
diffraction
The diffraction under different
patterns NaOH
of calcium
of calcium hydroxide,
hydroxide,
dosages.
calcite andTo C-S-H
our surprise, a noticeable
gel showed difference
only some betweeninthese
differences
differences mixtures
intensity was different
under that the NaOH
different
diffractionTo
dosages. patterns
To of AFt andaAFm
our surprise,
our surprise, showed difference
noticeable clear differences
difference between
betweenin intensity. The intensity
these mixtures was of that the
AFt was higher
diffraction in theofM11
patterns AFtpaste
and compared
AFm to theclear
showed otherdifferences
samples, whilein the intensity
intensity. The ofintensity
diffraction patterns of AFt and AFm showed clear differences in intensity. The intensity of
AFm was lower than others, indicating that the addition of 5 wt% NaOH promoted the
of
AFt AFt
waswas higher
higher in in
thethe M11paste
M11 pastecompared
comparedtotothe theother
othersamples,
samples, while
while the
the intensity of
formation of AFt and thus inhibited the formation of AFm, which was indicative of the
AFm was lower than others, indicating that the addition of 5 wt% NaOH promoted the
high strength of M11. Therefore, it could be drawn that the strength of M11 was improved
formation
formation
by the highofof AFt and
AFt
content and thus
thus inhibited
of AFt. inhibited the the formation
formation of of AFm,
AFm, which
which waswas indicative
indicative of of the
the
high
high strength
strength of of M11. Therefore, it
M11. Therefore, it could
could be drawn that
be drawn the strength
that the strength of M11 was
of M11 was improved
improved
by the high
by theAFthigh content
AFt content
AFt S of
of AFt.
S AFt.
C
Ht AFm AFm
CH CH
AFt AFt AFt SCH
S
C 8%
Ht AFm AFm
CH CH CH
5% 8%

3%
5%

1%
3%

0 10 20 30 40 50 60 70
2θ(°)
1%

0 10 20 30 40 50 60 70
2θ(°)

Figure 9. XRD analyses of pastes with different NaOH dosages at the curing age of 28 days. Ht:
hydrotalcite-like phase, CH: calcium hydroxide, S: C-S-H gel, C: calcium carbonate, AFt: ettringite,
AFm: calcium monosulfoaluminate.
 Buildings 2024, 14, x FOR PEER REVIEW 1

Figure 9. XRD analyses of pastes with different NaOH dosages at the curing age of 28 da
Buildings 2024, 14, 1681 12 of 19
hydrotalcite-like phase, CH: calcium hydroxide, S: C-S-H gel, C: calcium carbonate, AFt: ett
AFm: calcium monosulfoaluminate.

The results of XRD

The analysis
results of of XRD
hardened pasteofsamples
analysis hardened under different
paste curing
samples condi-
under different
tions at the curing stages at
conditions of the
3 days andstages
curing 28 days
of 3are
daysshown
and 28 in days
Figureare10. The products
shown in Figure of10. The pro
hydration of M15 to M17 were
of hydration of fairly
M15 to similar; C-S-Hfairly
M17 were gel, AFt and hydrotalcite-like
similar; C-S-H gel, AFt phasesand hydrotalci
were observedphases
with all mixtures. The main difference was that
were observed with all mixtures. The main difference the intensity wasofthat
C-S-H
the intensity
gel and AFt was higher in the M17 sample compared to the M16 at
S-H gel and AFt was higher in the M17 sample compared to the M16 at thethe curing time of curing t
3 days, which in turn was higher than that of the M15 sample. This indicated
3 days, which in turn was higher than that of the M15 sample. This indicated thatthat steam
curing promoted the production
curing promotedof the hydration products
production of and thus improved
hydration the compressive
products and thus improve
strength of M17. As the curing age of the samples increased to 28 days,
compressive strength of M17. As the curing age of the samples increased the intensity ofto 28 day
C-S-H gel and intensity
AFt in theofM15 and M16 increased, which meant that standard curing
C-S-H gel and AFt in the M15 and M16 increased, which meant that sta and
water curing promoted
curing andthe production
water of hydration
curing promoted the products
production at of
a later age. The
hydration XRD at a late
products
findings were well consistent with the strength development results.
The XRD findings were well consistent with the strength development results.

AFt AFt AFt S S (a) AFt AFt AFt S (b)

AFm C AFm C S
Ht AFm Ht AFmCH
CH CH CH CH CH

Steam curing Steam curing

Water curing
Water curing

Standard curing Standard curing

0 10 20 30 40 50 60 70 0 10 20 30 40 50 60 70
2θ(°) 2θ(°)

Figure
Figure 10. (a,b) XRD 10. (a,b)
analyses ofXRD analyses
pastes of pastescuring
under different under conditions
different curing
at theconditions
curing ageat
ofthe curing age of
3 days
and 28 days. Ht:and 28 days. Ht: hydrotalcite-like
hydrotalcite-like phase,
phase, CH: calcium CH: calcium
hydroxide, hydroxide,
S: C-S-H S: C-S-Hcarbonate,
gel, C: calcium gel, C: calcium carb
AFt: ettringite, AFm: calcium monosulfoaluminate.
AFt: ettringite, AFm: calcium monosulfoaluminate.

3.2.2. DSC/TG3.2.2. DSC/TG Analysis

Analysis
DSC/TG analysis DSC/TG analysis
provides a moreprovides
in-deptha more in-depth
description of description
these reaction of these reaction pro
products.
Figure 11 showedFigurethe11curves
showed of DSC/TG
the curves forofthe controlfor
DSC/TG sample and those
the control containing
sample and those cont
various carbidevarious
slag amounts
carbide at theamounts
slag age of 28atdays.
the ageAllofthe28samples
days. Allindicated
the samplesa similar
indicated a s
trend by showingtrendseveral main weight
by showing severallosses.
main The endothermic
weight losses. Thepeaks 23~230at◦ C
at about peaks
endothermic about 23~
corresponded corresponded
to the dehydration to theofdehydration
C-S-H, AFt of and AFm AFt
C-S-H, phasesand[45]
AFm and removal
phases [45] ofand remo
interlayer waterinterlayer
of the hydrotalcite-like phase, and these were difficult to distinguish.
water of the hydrotalcite-like phase, and these were difficult to distinguish Two
DSC peaks were clearly
DSC peaksvisible, and thevisible,
were clearly mass losses
and the of M1,
massM3, andofM5
losses M1,were
M3,5.83%,
and M5 6.62%,
were 5.83%,
and 7.62%, respectively,
and 7.62%, within this temperature
respectively, withinrange.
this The M3 and M5
temperature samples
range. Thedisplayed
M3 and M5 sa
a slightly higher weight loss
displayed a slightly 230 ◦ C than
before higher weighttheloss
control sample.
before 230 °CThis
thantrend of the result
the control sample. This
seemed to be similar to thatseemed
of the result obtained to by
be Rashad
similar toet that
al. [46], who found
obtained a larger
by Rashad weight
et al. loss found a
[46], who
before 200 ◦ C of the blast furnace slag sample activated by the addition of 15% limestone
weight loss before 200 °C of the blast furnace slag sample activated by the addition o
powder compared with the
limestone control
powder one. The
compared decomposition
with the control one. peakTheappearing
decompositionat aroundpeak appear
318 ◦ C could be assigned to the dehydroxilation of brucite-like layers of
around 318 °C could be assigned to the dehydroxilation of brucite-like lay hydrotalcite-like
phase, and the mass losses of M1,phase,
hydrotalcite-like M3, andandM5theinmass
this temperature
losses of M1,range were
M3, and M51.70%, 1.99%,
in this temperature
and 2.02%, respectively,
were 1.70%, showing
1.99%,higher contents
and 2.02%, of hydrotalcite-like
respectively, showingphasehigherwere generated
contents of hydrotalci
in the mixturesphase
with higher carbide slag
were generated addition.
in the mixtures Furthermore,
with higher◦acarbide
clearly increased peakFurtherm
slag addition.
and mass loss of M3 and M5 was observed between 370 and 460 C for the
clearly increased peak and mass loss of M3 and M5 was observed between 370 and decarbonation
of hydrotalcite-like phase
for the and the decomposition
decarbonation of Ca(OH)
of hydrotalcite-like 2 when
phase and increasing the carbide
the decomposition of Ca(OH)2
slag content inincreasing
the mixtures. the In addition,
carbide the
slag formation
content in of endothermic
the mixtures. peaks
In of M3 and
addition, the formati
◦ C was due to the decomposition of CaCO . In this temperature range, no
M5 at about 670endothermic peaks of M3 and M5 at about 670 3 °C was due to the decomposition of C
mass losses of M1 were found. The mass losses of M3 and M5 were 0.26% and 0.72%, which
In this temperature range, no mass losses of M1 were found. The mass losses of M
demonstrated that M5 had a high content of unreacted Ca(OH)2 and CaCO3 obtained by
carbonization. Therefore, it could be concluded that the addition of carbide slag increased
the content of hydrotalcite-like phase, Ca(OH)2 and CaCO3 and thus reduced the other
 Buildings 2024, 14, x FOR PEER REVIEW 14

Buildings 2024, 14, 1681 M5 were 0.26% and 0.72%, which demonstrated that M5 had a high content
13 of 19 of unrea
Ca(OH)2 and CaCO3 obtained by carbonization. Therefore, it could be concluded tha
addition of carbide slag increased the content of hydrotalcite-like phase, Ca(OH)
hydration products
CaCO of3 C-S-H andreduced
and thus AFt phases, whichhydration
the other was consistent with
products ofthe finding
C-S-H andofAFtthephases, w
XRD results. was consistent with the finding of the XRD results.
1.0 100 100
(a) 0.7 (b)
139℃ 417℃ 649℃
99

6.62%
132℃ 0.6 98
0.8

5.83%
DSC 98 DSC
0.5 759℃
771℃ 91℃ 339℃
0.6 815℃ 97 96
0.4 807℃
91℃

DSC(W/g)
DSC(W/g)
96

TG(%)
TG(%)
0.3
0.4 94
95 0.2

1.99%
94 0.1 92
0.2 TG

1.70%

1.14%
TG
93 0.0

0.26%
0.0 90
92 -0.1

0 200 400 600 800 1000 0 200 400 600 800 1000

Temperature(℃) Temperature(℃)
0.7 100
(c)
0.6 811℃ 98
651℃

7.62%
0.5 96
86℃ 337℃ DSC
0.4 425℃
94
143℃
DSC(W/g)

TG(%)
0.3
92

2.02%
0.2
90

2.22%

0.72%
0.1
TG
88
0.0
86
-0.1
0 200 400 600 800 1000

Temperature(℃)

Figureresults
Figure 11. Exemplary 11. Exemplary
of DSC/TG results of DSC/TG
analysis analysis
of paste of paste
(a) without (a) without
carbide carbide
slag; (b) slag; (b) with
with 10%
carbide
carbide slag; (c) with 20%slag; (c) with
carbide slag.20% carbide slag.

3.2.3. FTIR Analysis

3.2.3. FTIR Analysis
FTIR is powerful in determining
FTIR is powerful inthe structure ofthe
determining thestructure
functional groups
of the that build
functional groupsup that buil
the molecules. the
It enables the characterization
molecules. of the Si-O, Si-O-Si
It enables the characterization of theand
Si-O,O-H bonds,
Si-O-Si andwhich
O-H bonds, w
is useful to track the changes
is useful to track intheC-S-H gel and
changes AFt structures
in C-S-H gel and AFt as astructures
function asof avarious
function of va
factors [47,48]. factors
Figure [47,48].
12 shows the infrared spectra of pastes for the control
Figure 12 shows the infrared spectra of pastes for the controlsample and sample
those containing various carbidevarious
slag amounts −1
those containing carbideatslag
the amounts
age of 28at days. Theof
the age band at 957The
28 days. cmband at 957
was assigned towas theassigned
asymmetric to thestretching
asymmetric vibration of the
stretching Si-O bond
vibration in C-S-H
of the gels,inand
Si-O bond C-S-H gels
the band at 669the −1 corresponded
cmband to the Si-O-Si to bending vibration for C-S-H gels.
at 669 cm−1 corresponded the Si-O-Si bending vibration forThe
C-S-H gels
variation in these bands with
variation thebands
in these increase of the
with carbide slagof
increase amount
carbidefrom
slag 0% to 20%
amount was0%
from not
to 20% wa
evident as shown in Figure
evident 12d. Inin
as shown addition, the bands
Figure 12d. located the
In addition, between
bands3750 and 3000
located cm−13750 and
between
and near 1600 cm cm−−11 and
were assigned
near 1600 cm to−1O-H
werevibrations,
assigned to which can providewhich
O-H vibrations, evidence of the eviden
can provide
change in AFt [48]. −1 was broader in −1
the change in AFt [48]. This vibration band between 3750 and 3000 cm the
This vibration band between 3750 and 3000 cm was broad
M1 paste than in thethe
M1M3 andthan
paste M5 pastes,
in the M3 andandtheM5relative
pastes, area
andofthe
band decreased
relative area ofwith
bandthe decreased
increase of carbide
the slag, indicating
increase the reduction
of carbide in AFt content,
slag, indicating which was
the reduction in agreement
in AFt content, which w
with XRD and DSC/TG.
agreement with XRD and DSC/TG.

3.3. Microstructure Development

Figure 13 illustrates the representative SEM image of CAB pastes for the control sam-
ple and those containing various carbide slag content at the age of 28 days. The mixture of
anhydrous materials, hydrated phases and pores was clearly visible. The microstructure of
CAB pastes was significantly changed with the increase of carbide slag. The control sample
M1 showed a reasonable dense microstructure, which correlated with its good strength.
Partially replacing blast furnace slag with 10% carbide slag (M3) resulted in a relatively
dense microstructure, and there existed some unreacted carbide slag particles, thus decreas-
ing the compactness of M3. Further increasing the replacement level of blast furnace slag
with 20% carbide slag (M5) resulted in a loose and heterogeneous microstructure, and there
Buildings 2024, 14, 1681 14 of 19

were more unreacted carbide slag particles present, which could be distinguished
Buildings 2024, 14, x FOR PEER REVIEW
by their
15 of 21
sharp irregular morphology. As a result, the reduction in compressive strength increased.

450 (a) 450 O-H (b)

20: 80
400 400

350 350
20: 80
300 300

Transmittance (%)
Transmittance (%) 250 250 10: 90
10: 90
200 200

150 150 0: 100

100 100
0: 100
50 50

0 0

500 1000 1500 2000 2500 3000 3500 4000 2400 2600 2800 3000 3200 3400 3600 3800 4000

Wavenumber (cm-1) Wavenumber (cm-1)

250
260 O-H (c) Si-O (d)
Si-O-Si C-O
20: 80
240
200
220

200 20: 80
Transmittance (%)

Transmittance (%)
180 150
10: 90
160 10: 90
140 100
0: 100
120

100 50 0: 100
80

60 0
1400 1600 1800 2000 2200 2400 2600 400 600 800 1000 1200 1400 1600

Wavenumber (cm-1) Wavenumber (cm-1)

Figure 12. FTIR analysis of paste: (a) FTIR curves after 28 days of curing; (b) FTIR curves from 4000
Figure 12. FTIR analysis of paste: (a) FTIR curves after 28 days of curing; (b) FTIR curves from 4000
to 2500 cm−1; (c) FTIR curves from 2500 to 1500 cm−1; (d) FTIR curves from 1500 to 400 cm−1.
Buildings 2024, 14, x FOR PEER REVIEW 16 of 21
to 2500 cm−1 ; (c) FTIR curves from 2500 to 1500 cm−1 ; (d) FTIR curves from 1500 to 400 cm−1 .
3.3. Microstructure Development
Figure 13 illustrates the representative SEM image of CAB pastes for the control
sample and those containing various carbide slag content at the age of 28 days. The
mixture of anhydrous materials, hydrated phases and pores was clearly visible. The
microstructure of CAB pastes was significantly changed with the increase of carbide slag.
The control sample M1 showed a reasonable dense microstructure, which correlated with
its good strength. Partially replacing blast furnace slag with 10% carbide slag (M3)
resulted in a relatively dense microstructure, and there existed some unreacted carbide
slag particles, thus decreasing the compactness of M3. Further increasing the replacement
level of blast furnace slag with 20% carbide slag (M5) resulted in a loose and
heterogeneous microstructure, and there were more unreacted carbide slag particles
present, which could be distinguished by their sharp irregular morphology. As a result,
the reduction in compressive strength increased.

(a) (b)

(c)

Figure 13. SEMFigure 13. SEM images of CAB pastes at different carbide slag content: (a) without carbide slag; (b)
images of CAB pastes at different carbide slag content: (a) without carbide slag;
with 10% carbide slag; (c) with 20% carbide slag.
(b) with 10% carbide slag; (c) with 20% carbide slag.
The SEM micrographs of CAB pastes containing various NaOH dosage curing for 28
days are presented in Figure 14. There were significant differences in the morphologies
with different NaOH dosages. For sample M7, it was apparent that the edges of much of
the blast furnace slag and carbide slag particles were still clear, which meant low amounts
of hydration products were produced, which explained its relatively low compressive
strength. As the dosage of NaOH increased to 3 wt%, the unreacted slag particles became
small. In addition, some hydrated products were easily observed in the matrix, suggesting
that the increase of NaOH dosage promoted the hydration of blast furnace slag. With the
Buildings 2024, 14, 1681 15 of 19

The SEM micrographs of CAB pastes containing various NaOH dosage curing for
28 days are presented in Figure 14. There were significant differences in the morphologies
with different NaOH dosages. For sample M7, it was apparent that the edges of much of
the blast furnace slag and carbide slag particles were still clear, which meant low amounts
of hydration products were produced, which explained its relatively low compressive
strength. As the dosage of NaOH increased to 3 wt%, the unreacted slag particles became
small. In addition, some hydrated products were easily observed in the matrix, suggesting
that the increase of NaOH dosage promoted the hydration of blast furnace slag. With the
increase of NaOH, hydration products were more obvious and densify. M11 (Figure 14c)
showed a much dense microstructure, and no slag particles were observed. This was mainly
due to the large amount of AFt. The filling effect of AFt might play a role in reducing
the porosity of the matrix, which was related to the high compressive strength of M11.
For sample M13, large amounts of unreacted NaOH covered the surface of the hydration
Buildings 2024, 14, x FOR PEER REVIEW 17 of 21
products, which was detrimental to the compressive strength.

(a) (b)

(c) (d)
Figure
Figure 14.
14. SEM
SEM images
images of
of CAB
CAB pastes
pastes with
with different
different NaOH
NaOH content:
content: (a)
(a) with
with 11 wt%
wt% NaOH;
NaOH; (b)
(b) with
with
3 wt% NaOH; (c) with 5 wt% NaOH; (d) with 8 wt% NaOH.
3 wt% NaOH; (c) with 5 wt% NaOH; (d) with 8 wt% NaOH.

Figure 15 presents
Figure 15 presents the
theSEM
SEMimages
imagesofofCAB
CABpastes
pastesunder
underdifferent
different curing
curing conditions
conditions at
at the age of 28 days. The morphology of M17 was obviously different from
the age of 28 days. The morphology of M17 was obviously different from that of M15 that of M15
and
and
M16.M16. For sample
For sample M17,M17, it was
it was clearclear
that that the unreacted
the unreacted blastblast furnace
furnace slag slag and carbide
and carbide slag
slag
werewere obvious,
obvious, whichwhich explained
explained the decrease
the decrease of compressive
of compressive strength
strength at theatage
theofage of 28
28 days.
days. For samples M15 and M16, the hydration products increased, and unreacted blast
furnace slag and carbide slag were hardly observed in the matrix, indicating a relatively
dense microstructure. Therefore, it could be concluded that steam curing was not
conductive to the improvement of later strength.
Buildings 2024, 14, 1681 16 of 19

For samples M15 and M16, the hydration products increased, and unreacted blast furnace
slag and carbide slag were hardly observed in the matrix, indicating a relatively dense
microstructure. Therefore, it could be concluded that steam curing was not conductive
Buildings 2024, 14, x FOR PEER REVIEW 18 of to
21
the improvement of later strength.

(a) (b)

(c)
Figure 15.
Figure 15. SEM
SEMimages
imagesofofCAB
CAB pastes
pastes under
under different
different curing
curing conditions:
conditions: (a) standard
(a) standard curing;
curing; (b)
(b) water
water curing;
curing; (c) steam
(c) steam curing.curing.

4. Conclusions
In this study, the compressive strength and microstructure of carbide slag slag and
and alkali-
alkali-
activated blast furnace slag (CAB) pastes were investigated. The
pastes were investigated. The carbide carbide slag to blast
furnace slag ratio, alkali activator, and curing conditions have been shown to significantly
influence the
the compressive
compressivestrength
strengthandandmicrostructure
microstructure of CAB
of CABpastes. The The
pastes. following con-
following
clusions werewere
conclusions drawn. The compressive
drawn. strength
The compressive of CAB pastes
strength of CAB decreased with increasing
pastes decreased with
carbide slagcarbide
increasing substitution ratio and increased
slag substitution ratio andwith longer with
increased curing time.curing
longer After 28-days curing,
time. After 28-
the M1, M2, M3, M4, M5, and M6 mixes outperformed the 3-days
days curing, the M1, M2, M3, M4, M5, and M6 mixes outperformed the 3-days mix mix by 70.7%, 69.7%,
by
65.3%,
70.7%, 71.5%,
69.7%, 84.9%,
65.3%, and 56.8%,
71.5%, respectively,
84.9%, and 56.8%,and the compressive
respectively, and thestrength of the strength
compressive M2, M3,
M4,
of theM5,
M2,and
M3,M6 M4,mixes underperformed
M5, and the control mix
M6 mixes underperformed theM1 by 2.1%,
control 7.1%,
mix M1 by 9.2%, 9.8%,
2.1%, 7.1%,
and
9.2%,28.1%,
9.8%, respectively. Analysis revealed
and 28.1%, respectively. Analysisthatrevealed
the addition of carbide
that the additionslag reducedslag
of carbide the
content of C-S-H gel, decreased the intensity of the AFt phase, and promoted
reduced the content of C-S-H gel, decreased the intensity of the AFt phase, and promoted the formation
of
thehydrotalcite-like phase. Therefore,
formation of hydrotalcite-like the compressive
phase. Therefore, the strength of CAB strength
compressive pastes decreased
of CAB
with the increase of carbide slag, which was consistent with the findings
pastes decreased with the increase of carbide slag, which was consistent with of Seo
theetfindings
al. The
of Seo et al. The water-to-solid ratio of CAB pastes decreased slightly as the dosage of
NaOH increased, and there was also a decreasing trend in the setting time. The water-to-
solid ratio decreased to 0.49 at the dosage of 4% and then further decreased to 0.45 at the
dosage of 10%. The initial and final setting time of M7 was 89 min and 119 min, and it
decreased dramatically to 53 min and 89 min at the dosage of 5%. At last, it decreased
Buildings 2024, 14, 1681 17 of 19

water-to-solid ratio of CAB pastes decreased slightly as the dosage of NaOH increased, and
there was also a decreasing trend in the setting time. The water-to-solid ratio decreased
to 0.49 at the dosage of 4% and then further decreased to 0.45 at the dosage of 10%. The
initial and final setting time of M7 was 89 min and 119 min, and it decreased dramatically
to 53 min and 89 min at the dosage of 5%. At last, it decreased again but more steeply to
27 min and 68 min. The development of the strength with NaOH content increased first
and then decreased, and it reached the maximum of 24.8 MPa at 3 days and 36.3 MPa
at 7 days when the dosage of NaOH was 6%. The maximum compressive strengths of
43.3 MPa at 14 days and 44.5 MPa at 28 days were achieved when the dosage of NaOH was
5%. The high content of AFt was found to be related to the high strength, and its filling
effect played a role in reducing the porosity of the matrix. When curing at steam condition,
the compressive strength of 25.8 MPa was gained at 3 days, and this increased by 7.0% and
15.1% as the time increased from 7 days to 14 days, and then it decreased to 28.2 MPa at
28 days. Thus, it could be concluded that the steam curing enhanced the early strength
development of CAB pastes due to the high intensity of C-S-H gel and AFt produced,
but it was not conductive to the later strength development. The water curing enhanced
early strength development and contributed to the later strength as well. The compressive
strength of 23.3 MPa was gained at 3 days, and this increased by 16.3%, 24.0%, and 36.9%
at 7 days, 14 days, and 28 days, respectively. The standard curing was beneficial for later
strength but it was not unfavorable for the early strength development. The compressive
strength of 19.0 MPa was obtained at 3 days, and this increased by 51.6%, 60.5%, and
65.3% at 7 days, 14 days and 28 days, respectively. Thus, the water curing was suitable for
the strength development of CAB pastes. The compressive strengths of CAB pastes were
significantly high at 3 days, 7 days and 28 days relative to the previous similar study on fly
ash geopolymer activated by carbide slag.

Author Contributions: Methodology, Z.L. and J.W.; Formal analysis, Z.L.; Investigation, N.S., K.X.
(Kaiwang Xue), L.X., Y.R., Z.Y. and T.S.; Writing—original draft, K.X. (Kaidong Xu); Writing—review
& editing, Z.L.; Project administration, Z.L. All authors have read and agreed to the published version
of the manuscript.
Funding: This work was supported by the National College Student Innovation and Entrepreneurship
Training Program Project (202311765011); Program of Science and Technology Development of Henan
(232102320075, 222102320167).
Data Availability Statement: The original contributions presented in the study are included in the
article, further inquiries can be directed to the corresponding authors.
Conflicts of Interest: The authors declare no conflict of interest.

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