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Keywords: Portland cement showed a lower hydration rate and compressive strength development under lower temperature
CO2 curing environment. In this paper, a novel approach to improve compressive strength of cement paste at low temper
Low temperature ature by carbonation curing was put forwarded. The compressive strength of cement pastes under water-curing
Compressive strength
and CO2-cuirng at low temperature (5 ◦ C) are both investigated. X-ray diffractometer (XRD), Fourier transform
Microstructure
Calcium carbonate
infrared spectroscopy (FTIR) and Thermogravimetric analysis (TGA) were employed to analyze the phase
changes in carbonated cement pastes. Scanning electron microscope (SEM) with energy dispersive X-ray spec
troscopy (EDX) was adopted to examine the changes of morphologies and Mercury Intrusion Porosimeter (MIP)
was used to analyze the pore structure of carbonated cement pastes. The results showed that the 1 d and 28
d compressive strength of carbonated samples was 18.2 % and 54.1 % higher than the values in hydrated samples
at the corresponding ages. The 3 d compressive strength of carbonated sample was similar to the hydrated
samples cured at 28 d. Calcium silicate hydrate (C–S–H), ettringite and portlandite (Ca(OH)2) were formed in
hydrated sample, while calcium carbonate (CaCO3) and silica gel were generated in carbonated sample. The Ca
(OH)2 was increased from 7.9 % (1 d) to 11.3 % (28 d) in hydrated samples, while the CaCO3 was increased from
20.9 % at 1 d to 37.7 % at 28 d in carbonated samples. The total porosity was reduced from 19.7 % in hydrated
sample to 17.1 % in carbonated sample at 28 d. Furthermore, carbonation curing reduced the most probable pore
diameters in comparison to hydrated samples. The needle-like ettringite was observed in hydrated sample, while
typical prismatic calcite crystal was generated in carbonated samples. This paper confirmed that CO2 curing at
low temperature could be an effective and promising way to obtain rapid compressive strength improvement.
* Corresponding author at: School of Materials Science and Engineering, Henan Polytechnic University, Jiaozuo 454000, Henan, China (Z. Huo).
E-mail address: lubao@ycit.cn (B. Lu).
https://doi.org/10.1016/j.conbuildmat.2022.130128
Received 27 October 2022; Received in revised form 14 December 2022; Accepted 17 December 2022
Available online 22 December 2022
0950-0618/© 2022 Elsevier Ltd. All rights reserved.
L. Jiang et al. Construction and Building Materials 365 (2023) 130128
Table 1
Chemical and mineral composition of cement (wt. %).
SiO2 Al2O3 Fe2O3 CaO MgO SO3 f-CaO C3S C2S C3A C4AF
21.91 5.30 3.67 64.5 1.51 2.03 0.88 59.0 16.2 6.8 11.7
2. Experimental program
Fig. 1. Particle size distribution of Portland cement. 2.2. Specimen preparation and curing process
sodium nitrite, potassium carbonate, and sodium sulfate can facilitate The cement mortar and paste samples were prepared to preform
the hydration of cement, although they have different chemistry compressive strength and microstructure analysis, respectively. The
mechanisms [13,14]. However, the presence of extra alkali or sulfate in mortar samples with water to cement ratio of 0.4 and sand to cement
accelerator may cause durability problems, especially the steel corro mass ratio of 3.0 were mixed in a rotary mixer for 180 s and casted into
sion. The artificial heating is expensive and using the chemical admix 40 × 40 × 40 mm3 steel molds. While the paste samples with the same
tures resulted in corrosion [12,14,15]. water to binder ratio were prepared into 20 × 20 × 20 mm3 steel molds.
In recent decades, there have been growing research trend in CO2- It was to note that the molding process was finished at 5 ◦ C with relative
cured cement-based materials for their beneficial aspects of the promise humidity of 95 %. Afterwards all the specimens were placed into a
in CO2 sequestration, which would be of great significance on the CO2 chamber set at the given temperature of 5 ◦ C with the relative humidity
emissions reduction. It is well known that cementitious materials pol of 95 % and were demolded after 24 h. Then, particle pastes were shifted
ished up quickly on early strength and exhibited better durability to the CO2 chamber in which the temperature was 5 ◦ C, and the relative
properties subjected to accelerated carbonation due to the reaction be humidity and CO2 concentration were kept at 60 ± 5 % and 20 ± 2 %,
tween calcium silicates and CO2 [16–20]. Moreover, several studies also respectively. On the other hand, the other specimens were cured in a
have found that the early carbonation curing could accelerate early chamber with the temperature of 5 ◦ C and relative humidity of 95 % as
strength while maintaining subsequent hydration process of cement the control group.
pastes [21–23]. The formed calcium carbonate could react with alumi
nate to form calcium aluminate monocarboante, while the highly 2.3. Test methods
polymerization silica gel could react with portlandite to generate
C–S–H [23,24]. The re-hydration procedure applied after carbonation 2.3.1. Compressive strength
curing could increase early strength with maintain later strength. The compressive strength testing was carried out in accordance with
CO2 curing has made it possible that storing CO2 in cement-based EN 196–1-2005. Each batch comprised three specimens.
materials and using carbonate binders with low CO2 footprint would
have a profound impact on the evolution of the sustainable concrete 2.3.2. Phases analysis
industry [25–27]. Many studies have focused on the influence factors, A thin layer sample was cut off from the outer surface (0.2 mm) of the
including CO2 pressure, CO2 concentration, relative humidity, pre- cement paste and they were soaked in acetone solution to stop hydration
condition treatment, on the performance of CO2-cured cement-based process. Then these samples were ground into a powder which the
materials [28–30]. On the other hand, the carbonation behavior is fineness was small with particle size less than 45 μm and were dried in a
also relative with temperature change, which involving diffusion rate of vacuum oven at 50 ◦ C for 72 h. The collected cement paste powders were
CO2 and the solubility of free Ca2+ in cement [25]. The influence of used for XRD, FTIR and TG analysis.
room temperatures or high temperatures on the mechanical properties X ’PERT3 powder X-ray diffractometer from P Analytics was used for
and microstructure of carbonated cement samples were comprehensive XRD test. The 2θ scanning was performed between 5◦ and 65◦ with a
investigated [21,22,31]. However, the changed performance and scanning rate of 0.02◦ per step.
microstructure of CO2-cured cement samples at low temperature is still Approximately 1 mg of the powdered samples, as same with XRD
limited. Especially, the comparisons on the compressive strength and samples, was mixed with 100 mg of IR-grade KBr for 5 min. The mixture
microstructure of carbonated and hydrated cement samples at low was pressed into a thin disc which was the specimen, to be tested.
temperatures are not clear. Moreover, low temperatures resulted in a Through a Thermo-Scientific IS10 FTIR workstation, each specimen was
decrease in the early age hydration and mechanical strength. While it is scanned for 32 times at the resolution of 2 cm− 1.
not clear whether carbonation curing could be an approach to accelerate TG was performed using Netzsch STA 409 PC. Approximately 15 mg
2
L. Jiang et al. Construction and Building Materials 365 (2023) 130128
3
L. Jiang et al. Construction and Building Materials 365 (2023) 130128
Table 2
Typical wavenumbers of FTIR absorption for different chemicals.
Functional Wavenumbers (cm− 1)
groups
strong calcium carbonate peaks (2θ of 29.4◦ , 39.4◦ and 48.5◦ ) were
generated in CO2 cured samples, while no obvious portlandite and
ettringite patterns were detected in all aged carbonated samples, indi
cating portlandite and ettringite were consumed due to the carbonation
reactions [26]. Compared to carbonated samples, the hydrated samples
exhibited traces of calcium carbonate peak, which was attributed to Fig. 6. Content of CaCO3 and Ca(OH)2 based on TG-DTG curves at 5 ◦ C.
natural carbonation. Fig. 3 clearly showed that some C3S and C2S could
be found in the samples regard of CO2 or water curing. However, it was pastes as reported in the literature [37]. However, the band from 970
evident that C3S and C2S peaks were weaker in CO2 cured samples, cm− 1 in hydrated cement pastes shifted to 1060 cm− 1, corresponding to
suggesting carbonation reaction accelerated the consumption rate of C3S high polymerization of silica gel, in carbonated samples. The wave
and C2S, which polished up the strength of compression on carbonated number increased with the carbonation time duration, indicating the
cement mortar samples. aggregation performance of silica gel was improved [26,37]. Further
more, the band occurred at carbonated sample indicated CO2 curing
3.3. FTIR analysis could also improve the polymerization of silica gel at low temperature.
Fig. 4 displayed that the hydrated and carbonated cement pastes
Fig. 4 shows the FTIR spectra over the range of 4000–400 cm− 1 of the revealed a similar band at 1639 cm− 1 and 3446 cm-1because of the O–H
hydrated and carbonated paste samples at 5 ◦ C. The typical wave stretching in H2O [37]. In addition, a weak band corresponding to OH-
numbers of FTIR absorption for main chemicals in carbonation and stretching in Ca(OH)2 was detected at around 3644 cm− 1 in hydrated
hydration samples are summarized in Table 2 [34–36]. Generally, the samples [36]. while no obvious band at 3644 cm− 1 was found in
sharp vibrations at around 875 cm− 1, 714 cm− 1, 1080 cm− 1 and strong carbonated samples, suggesting carbonation reaction avoided the for
bond at 1420 cm− 1 are ascribed to C–O stretching, suggesting the mation of Ca(OH)2, which was similarly confirmed by XRD patterns.
CaCO3 was generated in cement pastes [37]. It was clear that the in
tensities of these three bands were stronger in carbonated pastes sam 3.4. TG-DTG analysis
ples, especially no obvious 714 cm− 1 band was detected in hydrated
samples, indicating more CaCO3 was formed due to the accelerated Fig. 5 shows the thermodynamic characteristics of different products
carbonation reactions, which was consist with XRD patterns in Fig. 3. in hydrated and carbonated pastes samples through the TG-DTG curves.
The detected relative weaker C–O stretching in hydrated pastes was due As expected, a mass loss in the range of 30 ◦ C − 200 ◦ C, corresponding to
to natural carbonation. Furthermore, compared to control samples, it the dehydration of C–S–H and ettringite, was observed in hydrated
can be seen that the band at 875 cm− 1 and 1420 cm− 1 became stronger sample at 1 d and it increased with the increasing hydration duration
and shaper in carbonated samples, indicating that the formed CaCO3 due to the more formation of C–S–H and ettringite products [39,40].
exhibited a better crystalline in accelerated carbonation reaction. Similar to hydrated sample, when the range of temperature was similar,
The band in range of 900–1100 cm− 1 are assigned to Si-O stretching a slightly mass loss was also detected in carbonated sample, which may
[37,38]. A Si-O stretching vibrations of Q2 sites was observed at around be attributed to the water loss of formed polymerized silica gel during
970 cm− 1 in hydrated sample and it exhibited no obvious change with carbonation curing [23,26]. An obvious steep mass occurred between
the hydration age, which was attributed to C–S–H in hydrated cement 400 ◦ C and 500 ◦ C, corresponding to the dehydration of Ca(OH)2, and it
4
L. Jiang et al. Construction and Building Materials 365 (2023) 130128
Fig. 7. Cumulative porosity and pore size distribution of hydrated and carbonated cement mortar at 28 d.
44.01
CaCO3 (%) = ΔM500◦ C− 950◦ C × × 100% (2)
100.09
5
L. Jiang et al. Construction and Building Materials 365 (2023) 130128
Fig. 9. SEM images and EDS spectrum of hydrated and carbonated samples at 1 d and 28 d.
can significantly promote compressive strength development even at and 9(b), obvious hydration products, including foil-like C–S–H gel,
low temperatures compared to the hydrated samples, which showed a platy Ca(OH)2 and need-like ettringite, could be recognized in hydrated
low compressive strength enhancement due to its low hydration rate at paste samples [33]. In addition, compared Fig. 9(a) with (b), the hy
low temperatures. drated paste at 28 d showed a denser microstructure, suggesting more
hydration products were formed prolonged hydration time. However,
3.6. SEM images the morphological evolution of carbonation products in the paste sam
ples under CO2 curing at different age are presented in Fig. 9(c)–(f). It
The SEM morphologies and EDS analysis of the hydrated and can be seen that no typical hydration products formed in carbonated
carbonated paste samples are presented in Fig. 9. As seen from Fig. 9(a) samples. Intensity, a large number of prismatic calcite crystal with the
6
L. Jiang et al. Construction and Building Materials 365 (2023) 130128
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Data availability
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Data will be made available on request.
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