High-Fluidization, Early Strength Cement Grouting Material Enhanced by Nano-SiO2: Formula and Mechanisms
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Methods
- According to the standard method [34], the beam samples with a size of 4 cm × 4 cm × 16 cm are prepared by curing the target age (1 day, 3 days, or 7 days).
- The sheet samples with a size of 2 cm × 2 cm × 1 cm are prepared by cutting the beam samples, and are put into absolute ethyl alcohol for seven days (the absolute ethyl alcohol must be replaced everyday).
- The treated sheet samples are prepared to cubic blocks with an approximate size of 1 cm × 1 cm × 1 cm after drying at 40 °C for 24 h.
- The SEM samples can be obtained via drying the cubic blocks at 40 °C for 48 h.
- The XRD, DSC, and FTIR samples can be obtained via drying the powder-grinded cubic blocks at 40 °C for 48 h. It should be noted that the powder must be passed through 80 μm, 150 μm, and 80 μm square sieves for the XRD, DSC, and FTIR tests, respectively.
3. Optimal Formula of High-Fluidization, Early Strength Cement Grouting Materials
3.1. Design of the Orthogonal Experiments
3.2. Orthogonal Experiment Analysis
3.3. The High-Fluidization, Early Strength Cement Grouting Enhanced by Nano-SiO2
4. Hydration Mechanisms of HCGA
4.1. Microstructure of HCGA
4.1.1. The Curing Age of 1-Day
4.1.2. The Curing Age of 3-Day
4.1.3. The Curing Age of 7-Day
4.2. X-ray Diffraction Analysis
4.3. Differential Scanning Calorimetry
4.4. Fourier Transform Infrared Spectroscopy
5. Conclusions
- The formula of the HCGA is water–cement ratio = 0.56, water-reducing agent = 1.2%, accelerating agent = 2.5%, expansion agent = 8%, and nano-SiO2 = 1%. The flexural and compressive strength of the HCGA at the curing age of 1 day is higher than 3.5 MPa and 12 MPa, respectively, while the fluidity and shrinkage rate is less than 11 s and 0.15%, respectively;
- Nano-SiO2 can significantly improve the flexural and compressive strength of the HCGA at an early curing age, while it will slightly weaken the fluidity. The enhancement of nano-SiO2 on the strength becomes weak when the content of nano-SiO2 exceeds 1%. Hence, considering economic costs, it is recommended that the recommended content of nano-SiO2 is 2%. In addition, the effects of nano-SiO2 decrease as the curing age increases, which has little significance at the curing age of 7 days. The mechanism of nano-SiO2 on the early strength of the HCGA is to accelerate the generation of CH crystals, to reach saturation at a faster rate and urge the CHS gels to generate early, while it is irrelevant to the AFt crystals;
- The types of hydration products of the HCGA are almost the same in the case of different curing ages and nano-SiO2 contents. Nano-SiO2 mainly takes part in the hydration reaction of tricalcium silicate, to improve the early strength in the HCGA, while it is irrelevant to the dicalcium silicate. The reaction period of nano-SiO2 is not fixed, which is related to the hydration rate. Compared to common cement-based materials, the effect of nano-SiO2 on the strength will occur ahead, as the hydration rate quickens in the HCGA (early strength materials).
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Stability | Setting Time (Min) | Flexural Strength (MPa) | Compressive Strength (MPa) | |||
---|---|---|---|---|---|---|
Initial Setting | Permanent Setting | 3d | 28d | 3d | 28d | |
Qualification | 170 | 210 | 5.7 | 8.9 | 30 | 53.6 |
Water Reduction (%) | Density (g/cm3) | Chloride Ion Content (%) | Alkali Content (%) | Bleeding Rate (%) | Compressive Strength Ratio (%) | |
---|---|---|---|---|---|---|
7d | 28d | |||||
21.2 | 1.031 | 0.21 | 3.5 | 30 | 150 | 135 |
Setting Time (Min) | Fineness (%) | Water Content (%) | 28d Compressive Strength Ratio (%) | 1d Compressive Strength (MPa) | |
---|---|---|---|---|---|
Initial Setting | Permanent Setting | ||||
2–3 | 8–10 | 11.6 | 1.7 | 75 | 9 |
Chemical Composition | Fineness | |||||
---|---|---|---|---|---|---|
Magnesium Oxide (%) | Water Content (%) | Total Alkali Content (%) | Chloride Ion (%) | Specific Surface Area (m2·kg−1) | 0.08 mm Material Retained (%) | 1.25 mm Material Retained (%) |
2.661 | 0.80 | 0.15 | 0.01 | 333 | 7.0 | 0.31 |
Particle Size (nm) | Specific Surface Area (m2/g) | Bulk Density (g/cm3) | Purity (%) | Appearance |
---|---|---|---|---|
15 | 600 | 0.21 | 99.8 | White grainy |
Level | Water–Cement Ratio | Expansion Agent (%) | Water-Reducing Agent (%) | Accelerating Agent (%) |
---|---|---|---|---|
I | 0.50 | 6 | 1.0 | 1.5 |
II | 0.53 | 7 | 1.2 | 2.0 |
III | 0.56 | 8 | 1.4 | 2.5 |
IV | 0.60 | 9 | 1.6 | 3.0 |
No. | Water–Cement Ratio | Expansion Agent (%) | Water-Reducing Agent (%) | Accelerating Agent (%) |
---|---|---|---|---|
1 | 0.50 | 6 | 1.0 | 1.5 |
2 | 0.50 | 7 | 1.2 | 2.0 |
3 | 0.50 | 8 | 1.4 | 2.5 |
4 | 0.50 | 9 | 1.6 | 3.0 |
5 | 0.53 | 8 | 1.0 | 2.0 |
6 | 0.53 | 9 | 1.2 | 1.5 |
7 | 0.53 | 6 | 1.4 | 3.0 |
8 | 0.53 | 7 | 1.6 | 2.5 |
9 | 0.56 | 9 | 1.0 | 2.5 |
10 | 0.56 | 8 | 1.2 | 3.0 |
11 | 0.56 | 7 | 1.4 | 1.5 |
12 | 0.56 | 6 | 1.6 | 2.0 |
13 | 0.60 | 7 | 1.0 | 3.0 |
14 | 0.60 | 6 | 1.2 | 2.5 |
15 | 0.60 | 9 | 1.4 | 2.0 |
16 | 0.60 | 8 | 1.6 | 1.5 |
No. | Flowing Time (s) | Flexural Strength (MPa) | Compressive Strength (MPa) | Shrinkage Rate (%) | |||||
---|---|---|---|---|---|---|---|---|---|
1-Day | 3-Day | 7-Day | 1-Day | 3-Day | 7-Day | 7-Day | 28-Day | ||
1 | 14.07 | 2.46 | 9.12 | 12.99 | 10.31 | 28.97 | 40.01 | 0.047 | 0.138 |
2 | 14.68 | 2.61 | 9.37 | 11.64 | 10.88 | 29.25 | 38.62 | 0.038 | 0.133 |
3 | 17.46 | 2.79 | 9.73 | 12.64 | 12.65 | 30.14 | 38.97 | 0.030 | 0.127 |
4 | 19.98 | 2.88 | 10.01 | 13.73 | 12.61 | 30.39 | 43.87 | 0.024 | 0.121 |
5 | 12.82 | 2.72 | 8.55 | 10.70 | 11.13 | 27.58 | 34.88 | 0.035 | 0.117 |
6 | 13.06 | 2.61 | 7.79 | 10.68 | 9.62 | 26.23 | 35.67 | 0.027 | 0.111 |
7 | 14.67 | 3.05 | 8.89 | 11.62 | 12.05 | 28.59 | 36.02 | 0.041 | 0.139 |
8 | 14.34 | 2.81 | 8.17 | 11.31 | 10.11 | 27.26 | 37.00 | 0.030 | 0.126 |
9 | 9.22 | 3.11 | 8.07 | 10.86 | 11.01 | 26.19 | 34.91 | 0.021 | 0.101 |
10 | 10.84 | 3.40 | 8.21 | 10.01 | 10.46 | 26.67 | 34.39 | 0.017 | 0.107 |
11 | 11.09 | 2.76 | 7.21 | 9.12 | 9.29 | 25.68 | 31.4 | 0.022 | 0.112 |
12 | 11.76 | 2.91 | 7.28 | 9.96 | 9.38 | 26.01 | 35.39 | 0.031 | 0.119 |
13 | 8.78 | 2.67 | 6.17 | 8.24 | 8.97 | 21.76 | 28.76 | 0.027 | 0.109 |
14 | 9.96 | 2.31 | 5.48 | 7.06 | 7.29 | 21.75 | 28.70 | 0.026 | 0.106 |
15 | 9.85 | 2.21 | 5.25 | 6.94 | 6.11 | 20.69 | 26.54 | 0.010 | 0.096 |
16 | 10.46 | 2.03 | 5.01 | 6.54 | 5.68 | 20.67 | 27.4 | 0.008 | 0.096 |
Index | Water–Cement Ratio | Water-Reducing Agent | Accelerating Agent | Expansion Agent | ||
---|---|---|---|---|---|---|
Fluidity (Flowing time) (s) | Average value | level I | 16.55 | 11.22 | 12.17 | 12.62 |
level II | 13.72 | 11.95 | 12.28 | 13.09 | ||
level III | 10.73 | 13.27 | 12.57 | 12.90 | ||
level IV | 9.76 | 14.14 | 13.58 | 13.03 | ||
Range | 6.79 | 2.91 | 1.40 | 0.47 | ||
1-day flexural strength (MPa) | Average value | level I | 2.69 | 2.74 | 2.47 | 2.68 |
level II | 2.80 | 2.73 | 2.61 | 2.71 | ||
level III | 3.04 | 2.70 | 2.68 | 2.74 | ||
level IV | 2.30 | 2.66 | 3.00 | 2.70 | ||
Range | 0.74 | 0.09 | 0.54 | 0.06 | ||
1-day compressive strength (MPa) | Average value | level I | 11.61 | 10.36 | 8.73 | 9.76 |
level II | 10.73 | 9.72 | 9.37 | 10.17 | ||
level III | 10.04 | 10.02 | 9.86 | 9.98 | ||
level IV | 7.01 | 9.44 | 11.02 | 9.83 | ||
Range | 4.60 | 0.91 | 2.30 | 0.41 | ||
3-day flexural strength (MPa) | Average value | level I | 9.56 | 7.98 | 7.28 | 7.69 |
level II | 8.35 | 7.77 | 7.61 | 8.10 | ||
level III | 7.69 | 7.77 | 7.72 | 7.88 | ||
level IV | 5.48 | 7.62 | 8.32 | 7.78 | ||
Range | 4.08 | 0.36 | 1.04 | 0.40 | ||
3-day compressive strength (MPa) | Average value | level I | 29.69 | 26.13 | 25.39 | 26.33 |
level II | 27.41 | 26.01 | 25.88 | 25.99 | ||
level III | 26.13 | 26.28 | 26.10 | 26.27 | ||
level IV | 21.22 | 26.08 | 26.85 | 25.88 | ||
Range | 8.47 | 0.27 | 1.47 | 0.46 | ||
7-day flexural strength (MPa) | Average value | level I | 12.75 | 10.70 | 9.83 | 10.41 |
level II | 11.08 | 10.02 | 9.81 | 10.61 | ||
level III | 9.99 | 10.08 | 10.25 | 9.97 | ||
level IV | 7.20 | 10.39 | 10.90 | 10.55 | ||
Range | 5.56 | 0.68 | 1.09 | 0.64 | ||
7-day compressive strength (MPa) | Average value | level I | 40.37 | 34.64 | 33.62 | 35.03 |
level II | 35.89 | 34.40 | 33.86 | 35.23 | ||
level III | 34.02 | 33.23 | 34.51 | 33.91 | ||
level IV | 27.85 | 35.92 | 35.76 | 35.25 | ||
Range | 12.51 | 2.68 | 2.14 | 1.34 | ||
7-day shrinkage rate (%) | Average value | level I | 0.035 | 0.033 | 0.026 | 0.036 |
level II | 0.033 | 0.028 | 0.029 | 0.030 | ||
level III | 0.023 | 0.026 | 0.027 | 0.023 | ||
level IV | 0.018 | 0.023 | 0.027 | 0.021 | ||
Range | 0.017 | 0.009 | 0.003 | 0.016 | ||
28-day shrinkage rate (%) | Average value | level I | 0.130 | 0.116 | 0.114 | 0.126 |
level II | 0.123 | 0.115 | 0.116 | 0.122 | ||
level III | 0.110 | 0.119 | 0.115 | 0.112 | ||
level IV | 0.102 | 0.116 | 0.119 | 0.107 | ||
Range | 0.028 | 0.004 | 0.005 | 0.018 |
Property Index | Water–Cement Ratio | Expansion Agent | Water-Reducing Agent | Accelerating Agent |
---|---|---|---|---|
Fluidity (flow time) | ✔✔ | ✔ | ✔ | |
1-day flexural strength | ✔✔ | ✔ | ||
1-day compressive strength | ✔✔ | ✔ | ||
3-day flexural strength | ✔✔ | |||
3-day compressive strength | ✔✔ | |||
7-day flexural strength | ✔✔ | |||
7-day compressive strength | ✔✔ | |||
7-day dry-shrinkage ratio | ✔✔ | ✔✔ | ✔ | |
28-day dry-shrinkage ratio | ✔✔ | ✔ |
No. | Water–Cement Ratio | Water-Reducing Agent | Accelerating Agent | Expansion Agent |
---|---|---|---|---|
Y-1 | 0.53 | 1.0% | 2.0% | 9% |
Y-2 | 0.53 | 1.0% | 2.5% | 9% |
Y-3 | 0.56 | 1.2% | 2.0% | 8% |
Y-4 | 0.56 | 1.2% | 2.5% | 8% |
No. | Fluidity (s) | Flexural Strength (MPa) | Compressive Strength (MPa) | Shrinkage Rate (%) | |||||
---|---|---|---|---|---|---|---|---|---|
1-Day | 3-Day | 7-Day | 1-Day | 3-Day | 7-Day | 7-Day | 28-Day | ||
Y-1 | 12.86 | 2.69 | 8.35 | 11.10 | 10.82 | 27.11 | 35.89 | 0.018 | 0.121 |
Y-2 | 13.11 | 2.89 | 8.46 | 11.21 | 11.39 | 27.29 | 35.91 | 0.027 | 0.118 |
Y-3 | 10.01 | 3.13 | 8.06 | 10.35 | 10.29 | 25.86 | 34.17 | 0.019 | 0.101 |
Y-4 | 10.38 | 3.43 | 8.18 | 10.66 | 10.91 | 26.02 | 34.38 | 0.021 | 0.108 |
Requirement | 9–13 | -- | -- | ≥ 2 | -- | -- | 10–30 | -- | <0.5 |
Nona-SiO2 Content | Fluidity (s) | Flexural Strength (MPa) | Compressive Strength (MPa) | Shrinkage Rate (%) | |||||
---|---|---|---|---|---|---|---|---|---|
1-Day | 3-Day | 7-Day | 1-Day | 3-Day | 7-Day | 7-Day | 28-Day | ||
0% | 10.38 | 3.43 | 8.18 | 10.66 | 10.91 | 26.02 | 34.38 | 0.019 | 0.108 |
1% | 10.61 | 3.77 | 8.46 | 10.68 | 12.18 | 27.16 | 35.01 | 0.017 | 0.111 |
2% | 11.29 | 3.98 | 8.59 | 10.76 | 13.01 | 28.38 | 34.69 | 0.021 | 0.108 |
3% | 12.89 | 4.11 | 8.68 | 10.61 | 14.68 | 29.02 | 34.61 | 0.019 | 0.113 |
Standard | 9–13 | -- | -- | ≥ 2 | -- | -- | 10–30 | -- | <0.5 |
Nona-SiO2 Content | COV (%) | ||||||||
---|---|---|---|---|---|---|---|---|---|
Fluidity | Flexural Strength | Compressive Strength | Shrinkage Rate | ||||||
1-Day | 3-Day | 7-Day | 1-Day | 3-Day | 7-Day | 7-Day | 28-Day | ||
0% | 5.29 | 8.63 | 3.31 | 4.38 | 7.48 | 4.88 | 3.29 | 7.38 | 2.31 |
1% | 7.31 | 3.52 | 4.87 | 3.45 | 4.62 | 6.20 | 5.13 | 10.89 | 4.98 |
2% | 4.26 | 5.96 | 6.66 | 2.96 | 9.04 | 6.34 | 5.67 | 5.02 | 3.70 |
3% | 8.60 | 7.29 | 5.88 | 3.77 | 5.11 | 3.07 | 4.74 | 9.97 | 2.11 |
Requirement | <10 | <10 | <15 |
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Ren, J.; Zhao, Z.; Xu, Y.; Wang, S.; Chen, H.; Huang, J.; Xue, B.; Wang, J.; Chen, J.; Yang, C. High-Fluidization, Early Strength Cement Grouting Material Enhanced by Nano-SiO2: Formula and Mechanisms. Materials 2021, 14, 6144. https://doi.org/10.3390/ma14206144
Ren J, Zhao Z, Xu Y, Wang S, Chen H, Huang J, Xue B, Wang J, Chen J, Yang C. High-Fluidization, Early Strength Cement Grouting Material Enhanced by Nano-SiO2: Formula and Mechanisms. Materials. 2021; 14(20):6144. https://doi.org/10.3390/ma14206144
Chicago/Turabian StyleRen, Jiaolong, Zedong Zhao, Yinshan Xu, Siyuan Wang, Haiwei Chen, Jiandong Huang, Boxin Xue, Jian Wang, Jingchun Chen, and Chengxu Yang. 2021. "High-Fluidization, Early Strength Cement Grouting Material Enhanced by Nano-SiO2: Formula and Mechanisms" Materials 14, no. 20: 6144. https://doi.org/10.3390/ma14206144