Experimental Characterization and Multi-Factor Modelling to Achieve Desired Flow, Set and Strength of N-A-S-H Geopolymers
Abstract
:1. Introduction
2. Experimental Program
2.1. Materials and Mix Proportions
2.2. Sample Preparation
2.3. Test Protocols
3. Experimental Results and Analyses
3.1. Rheology of Fresh Geopolymer Mixtures
3.2. Temperature Evolution during Setting Process
3.3. X-ray Diffraction (XRD) and Thermogravimetric Analysis (TGA)
3.4. Fourier Transform Infrared Spectroscopy (FTIR)
3.5. Scanning Electron Micrographs
3.6. Workability, Final Setting Time and Compressive Strength
3.7. Sensitivity Analysis
4. Establishment of Multi-Factor Models
4.1. Find the Relationship between Variables and Predicted Outcomes
4.2. Determine Regression Coefficients for Multi-Factor Models
4.3. Model Justification
5. Further Discussion
6. Conclusions
- (1).
- An increase in the Na2O/Al2O3 or H2O/Na2O ratio reduces the viscosity of the fresh geopolymer mixture due to a corresponding increase in the liquid-to-solid ratio. There was an accompanying drop in the yield shear stress. Together, this leads to a greater flowability. However, there exists an optimum SiO2/Al2O3 ratio to obtain the lowest viscosity. Whereas, at lower values, the system is dominated by sodium silicate, once this ratio exceeds 3.2, the liquid-to-solid ratio dominates and eventually raises the flowability of the system;
- (2).
- In N-A-S-H geopolymers, the setting time is associated with the exothermicity during the geopolymerization, which was found most sensitive to the SiO2/Al2O3 ratio. The mixture made with a SiO2/Al2O3 ratio of about 2.8 registered the highest peak temperature and the fastest temperature rise, both of which coincide with its fastest setting time;
- (3).
- A deficient SiO2/Al2O3 ratio and an excessive Na2O/Al2O3 ratio will, in either case, deter geopolymerization. Additionally, they promote significant zeolite formation. This was evident from the reduced amorphicity in XRD, a wider but much lower DTG peak assigned to depolymerization of N-A-S-H in TGA, and also a smaller peak area ascribed to the Si-O-T band in the N-A-S-H framework in FTIR. The H2O/Na2O ratio at its optimum value, found to be 9~10 here, led to the highest amorphicity and degree of polycondensation;
- (4).
- The proposed multi-factor models capture the effect of each oxide component in the mixture design upon the possible flow, final setting time and compressive strength. When the mutual interactions between the different oxide ratios are considered, the coefficient of determination for flow improved from 0.79 to 0.92, for setting time, from 0.87 to 0.95 and from 0.83 to 0.88 for the compressive strength. More importantly, these proposed models may serve as a predictive tool to conduct and validate mixture design for N-A-S-H geopolymers with varying priorities upon workability, final set and compressive strength;
- (5).
- A satisfactory combination of compositional ratios to simultaneously achieve the desired workability, final set and compressive strength may fall within SiO2/Al2O3 = 2.8~3.6, Na2O/Al2O3 = 0.75~1.0 and H2O/Na2O = 9~10. The workability of the fresh N-A-S-H mixture is most sensitive to the H2O/Na2O ratio, while the setting time is predominantly governed by the SiO2/Al2O3 ratio. The compressive strength is sensitive to the H2O/Na2O ratio and, to a lesser extent, the SiO2/Al2O3 ratio as well.
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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SiO2 | Al2O3 | TiO2 | Fe2O3 | P2O5 | Na2O | K2O | CaO |
---|---|---|---|---|---|---|---|
53.8% | 43.8% | 0.9% | 0.5% | 0.4% | 0.3% | 0.2% | 0.1% |
SiO2/Al2O3 (Molar Ratio) | Na2O/Al2O3 (Molar Ratio) | H2O/Na2O (Molar Ratio) | Metakaolin (g) | Sodium Silicate (g) | NaOH Pellet (g) | Water (g) | Liquid-to-Solid |
---|---|---|---|---|---|---|---|
2.1 | 1.15 | 11 | 500 | 6.63 | 196.86 | 484.96 | 1.377 |
2.8 | 1.15 | 11 | 500 | 320.98 | 160.76 | 400.76 | 1.540 |
3.6 | 1.15 | 11 | 500 | 680.23 | 119.50 | 63.96 | 1.727 |
4.0 | 1.15 | 11 | 500 | 837.41 | 104.89 | 0 | 1.885 |
2.8 | 0.75 | 11 | 500 | 320.98 | 92.02 | 118.37 | 1.063 |
2.8 | 1.00 | 11 | 500 | 320.98 | 134.98 | 224.70 | 1.361 |
2.8 | 1.30 | 11 | 500 | 320.98 | 186.54 | 352.29 | 1.720 |
2.8 | 1.00 | 8 | 500 | 320.98 | 134.98 | 108.71 | 1.129 |
2.8 | 1.00 | 9 | 500 | 320.98 | 134.98 | 147.37 | 1.207 |
2.8 | 1.00 | 10 | 500 | 320.98 | 134.98 | 186.04 | 1.284 |
2.8 | 1.00 | 11 | 500 | 320.98 | 134.98 | 224.70 | 1.361 |
2.8 | 1.00 | 12 | 500 | 320.98 | 134.98 | 263.37 | 1.439 |
SiO2/Al2O3 (Molar Ratio) | Na2O/Al2O3 (Molar Ratio) | H2O/Na2O (Molar Ratio) | Metakaolin (g) | Sodium Silicate (g) | NaOH Pellet (g) | Water (g) | Liquid-to-Solid |
---|---|---|---|---|---|---|---|
2.4 | 1.40 | 16 | 50 | 14.14 | 22.43 | 77.77 | 2.287 |
2.8 | 1.40 | 16 | 50 | 32.10 | 20.37 | 66.55 | 2.380 |
3.2 | 1.40 | 16 | 50 | 50.06 | 18.31 | 55.32 | 2.474 |
3.5 | 1.40 | 16 | 50 | 63.53 | 16.76 | 46.90 | 2.544 |
3.6 | 1.40 | 16 | 50 | 68.02 | 16.25 | 44.09 | 2.556 |
2.8 | 1.10 | 16 | 50 | 32.10 | 15.22 | 47.99 | 1.906 |
2.8 | 1.25 | 16 | 50 | 32.10 | 17.79 | 57.27 | 2.143 |
2.8 | 1.40 | 16 | 50 | 32.10 | 20.37 | 66.55 | 2.380 |
2.8 | 1.40 | 16 | 50 | 32.10 | 20.37 | 44.90 | 1.947 |
2.8 | 1.40 | 16 | 50 | 32.10 | 20.37 | 55.72 | 2.164 |
2.8 | 1.40 | 16 | 50 | 32.10 | 20.37 | 66.55 | 2.380 |
SiO2/Al2O3 (Molar Ratio) | Na2O/Al2O3 (Molar Ratio) | H2O/Na2O (Molar Ratio) | Flow Diameter (mm) | Final Setting Time (min) | Compressive Strength (MPa) |
---|---|---|---|---|---|
2.1 | 0.95 | 11 | 152.3 | - | - |
2.4 * | 203.5 | - | - | ||
2.8 | 257.3 | - | - | ||
3.1 | 261.0 | - | - | ||
2.1 | 1.15 | 11 | - | 480 | 11.78 |
2.8 * | - | 190 | 32.71 | ||
3.6 | - | 360 | 40.23 | ||
4.0 | - | 740 | 46.19 | ||
2.1 | 0.75 | 11 | 101.5 | - | - |
0.95 * | 152.3 | - | - | ||
1.15 | 196.9 | - | - | ||
1.25 | 247.7 | - | - | ||
2.8 | 0.75 | 11 | - | 195 | 47.54 |
1.00 * | - | 180 | 29.53 | ||
1.15 | - | 190 | 32.71 | ||
1.30 | - | 210 | 19.24 | ||
2.8 | 1.00 | 8 | 225.1 | 160 | 39.83 |
9 * | 239.5 | 130 | 43.03 | ||
10 | 254.7 | 165 | 50.68 | ||
11 | 261.0 | 180 | 29.53 |
SiO2/Al2O3 | Na2O/Al2O3 | H2O/Na2O | L/S | Tested Flow (mm) | Predicted Flow (mm) | Tested Set (min) | Predicted Set (min) | Tested Strength (MPa) | Predicted Strength (MPa) |
---|---|---|---|---|---|---|---|---|---|
2.1 | 0.75 | 11 | 0.899 | 101.5 ± 1.2 | 107.8 | 140 | 144 | 17.3 ± 2.9 | 17.6 |
2.1 | 0.95 | 11 | 1.138 | 152.3 ± 1.7 | 167.8 | 185 | 172 | 11.6 ± 0.9 | 12.7 |
2.2 | 0.75 | 11 | 0.923 | 109.3 ± 0.7 | 126.6 | 100 | 131 | 21.3 ± 2.8 | 22.2 |
2.3 | 1.00 | 9 | 1.090 | 147.1 ± 1.0 | 154.1 | 115 | 124 | 33.0 ± 0.8 | 27.5 |
2.3 | 1.00 | 10 | 1.167 | 185.5 ± 0.8 | 188.0 | 130 | 131 | 23.8 ± 3.3 | 23.4 |
2.3 | 1.00 | 12 | 1.322 | 225.4 ± 0.2 | 231.3 | 160 | 179 | 10.3 ± 1.2 | 14.5 |
2.3 | 1.00 | 14 | 1.476 | 255.7 ± 0.5 | 241.7 | 220 | 269 | 8.9 ± 0.5 | 6.9 |
2.4 | 0.75 | 11 | 0.969 | 172.9 ± 0.2 | 160.1 | 120 | 123 | 30.8 ± 2.2 | 30.7 |
2.4 | 0.95 | 11 | 1.208 | 203.5 ± 0.4 | 210.0 | 135 | 129 | 20.6 ± 0.9 | 24.0 |
2.4 | 1.15 | 11 | 1.447 | 285.9 ± 0.5 | 280.6 | 180 | 184 | 20.2 ± 1.7 | 17.7 |
2.4 | 0.80 | 11 | 1.029 | 189.6 ± 1.8 | 170.7 | 85 | 120 | 27.5 ± 2.9 | 29.0 |
2.4 | 1.00 | 11 | 1.268 | 242.7 ± 0.2 | 225.7 | 140 | 139 | 20.3 ± 2.0 | 22.4 |
2.4 | 1.20 | 11 | 1.507 | 307.3 ± 0.1 | 301.5 | 195 | 205 | 18.7 ± 1.8 | 16.2 |
2.6 | 0.88 | 11.5 | 1.210 | 247.2 ± 1.8 | 224.2 | 120 | 136 | 30.3 ± 3.2 | 29.8 |
2.7 | 0.90 | 9 | 1.086 | 157.1 ± 1.9 | 173.9 | 90 | 128 | 39.2 ± 1.0 | 45.2 |
2.7 | 0.90 | 10 | 1.149 | 180.7 ± 1.0 | 204.6 | 110 | 126 | 43.8 ± 2.7 | 40.5 |
2.7 | 0.90 | 12 | 1.288 | 215.7 ± 1.0 | 245.5 | 165 | 155 | 29.7 ± 2.6 | 29.4 |
2.7 | 0.90 | 14 | 1.427 | 238.9 ± 0.7 | 256.9 | 235 | 227 | 15.1 ± 1.3 | 19.8 |
2.8 | 0.95 | 11 | 1.302 | 257.3 ± 0.7 | 248.2 | 165 | 149 | 30.4 ± 0.2 | 35.6 |
2.8 | 1.15 | 11 | 1.540 | 285.7 ± 0.2 | 305.2 | 190 | 171 | 32.7 ± 1.9 | 29.4 |
2.8 | 0.75 | 11 | 1.063 | 223.8 ± 1.6 | 211.9 | 195 | 172 | 47.5 ± 3.7 | 43.9 |
2.8 | 0.80 | 11 | 1.122 | 232.0 ± 0.8 | 219.0 | 155 | 162 | 43.6 ± 3.3 | 41.7 |
2.8 | 1.00 | 11 | 1.361 | 261.0 ± 0.5 | 260.6 | 180 | 150 | 29.5 ± 1.0 | 33.9 |
2.8 | 1.20 | 11 | 1.600 | 321.5 ± 0.8 | 322.7 | 195 | 184 | 28.0 ± 2.0 | 28.2 |
2.8 | 1.00 | 8 | 1.129 | 225.1 ± 0.2 | 170.8 | 160 | 182 | 39.8 ± 2.6 | 46.0 |
2.8 | 1.00 | 9 | 1.207 | 239.5 ± 0.3 | 209.0 | 130 | 162 | 43.0 ± 0.7 | 45.2 |
2.8 | 1.00 | 10 | 1.284 | 254.7 ± 0.9 | 238.9 | 165 | 151 | 50.7 ± 2.2 | 39.4 |
2.8 | 1.00 | 12 | 1.439 | 285.9 ± 0.2 | 274.0 | 185 | 160 | 28.8 ± 1.3 | 29.1 |
2.9 | 0.99 | 11 | 1.368 | 287.3 ± 0.1 | 263.7 | 145 | 167 | 39.8 ± 0.6 | 36.8 |
3.1 | 0.75 | 11 | 1.133 | 224.9 ± 0.6 | 237.1 | 315 | 267 | 53.4 ± 2.8 | 50.8 |
3.1 | 0.95 | 11 | 1.372 | 261.0 ± 0.7 | 263.3 | 240 | 221 | 32.5 ± 1.1 | 41.7 |
3.2 | 0.75 | 11 | 1.156 | 227.8 ± 1.2 | 243.0 | 380 | 310 | 49.0 ± 0.9 | 52.6 |
3.2 | 0.80 | 11 | 1.216 | 235.7 ± 0.9 | 246.7 | 350 | 293 | 49.1 ± 0.6 | 49.8 |
3.2 | 0.80 | 12.7 | 1.321 | 261.0 ± 1.7 | 271.2 | 365 | 343 | 46.5 ± 2.1 | 38.7 |
3.2 | 1.00 | 11 | 1.455 | 261.0 ± 1.1 | 274.7 | 235 | 249 | 50.6 ± 0.9 | 41.5 |
3.3 | 1.02 | 10.5 | 1.466 | 253.8 ± 0.7 | 270.8 | 260 | 296 | 48.0 ± 2.3 | 44.9 |
3.3 | 0.95 | 11 | 1.418 | 271.7 ± 0.2 | 267.1 | 290 | 297 | 37.3 ± 2.4 | 44.6 |
3.3 | 1.00 | 9 | 1.323 | 232.5 ± 2.1 | 231.6 | 305 | 339 | 50.8 ± 2.6 | 56.8 |
3.3 | 1.00 | 10 | 1.401 | 241.7 ± 1.7 | 257.4 | 295 | 309 | 59.9 ± 1.6 | 49.3 |
3.5 | 1.00 | 11 | 1.482 | 293.0 ± 0.4 | 279.8 | 350 | 383 | 50.0 ± 0.8 | 49.3 |
3.6 | 0.85 | 13 | 1.501 | 285.9 ± 0.5 | 273.3 | 520 | 527 | 40.2 ± 3.2 | 39.0 |
3.6 | 0.85 | 10 | 1.303 | 236.9 ± 0.7 | 236.2 | 430 | 485 | 51.5 ± 0.5 | 58.6 |
3.6 | 0.95 | 11.5 | 1.525 | 289.5 ± 0.5 | 268.2 | 415 | 445 | 41.0 ± 1.9 | 43.9 |
2.4 | 1.30 | 11 | 1.626 | / | / | 260 | 255 | 11.9 ± 0.3 | 13.2 |
2.8 | 1.30 | 11 | 1.720 | / | / | 210 | 218 | 19.2 ± 0.6 | 26.1 |
3.2 | 1.30 | 11 | 1.813 | / | / | 265 | 267 | 41.8 ± 1.7 | 36.2 |
3.6 | 1.15 | 11 | 1.727 | / | / | 360 | 407 | 40.2 ± 1.3 | 42.9 |
3.8 | 0.95 | 13 | 1.682 | / | / | 555 | 558 | 40.3 ± 3.5 | 38.7 |
4.0 | 1.20 | 12 | 1.973 | / | / | 475 | 533 | 42.1 ± 0.4 | 44.4 |
4.0 | 1.15 | 11 | 1.885 | / | / | 740 | 621 | 46.2 ± 3.3 | 45.3 |
SiO2/Al2O3 | Na2O/Al2O3 | H2O/Na2O | L/S | Tested Flow (mm) | Predicted Flow (mm) | Tested Set (min) | Predicted Set (min) | Tested Strength (MPa) | Predicted Strength (MPa) |
---|---|---|---|---|---|---|---|---|---|
2.2 | 0.85 | 11 | 1.042 | 143.53 ± 2.5 | 152.3 | 125 | 136 | 16.7 ± 1.3 | 19.6 |
2.6 | 0.90 | 10 | 1.126 | 201.40 ± 0.4 | 194.2 | 120 | 115 | 36.0 ± 3.2 | 37.4 |
2.7 | 1.00 | 11 | 1.275 | 240.87 ± 0.7 | 251.5 | 190 | 141 | 32.7 ± 2.4 | 35.5 |
3.0 | 0.85 | 11 | 1.229 | 240.54 ± 0.5 | 242.2 | 245 | 205 | 45.8 ± 3.3 | 44.0 |
3.4 | 0.90 | 10 | 1.312 | 243.13 ± 0.8 | 241.7 | 350 | 361 | 49.5 ± 1.7 | 54.6 |
3.4 | 0.80 | 10 | 1.201 | 214.90 ± 0.8 | 230.7 | 395 | 376 | 60.4 ± 4.3 | 59.5 |
3.4 | 1.00 | 10 | 1.424 | 263.03 ± 0.4 | 257.3 | 360 | 357 | 57.5 ± 2.7 | 50.5 |
3.4 | 1.20 | 10 | 1.648 | 335.14 ± 0.2 | 303.1 | 335 | 382 | 51.1 ± 2.1 | 45.6 |
3.4 | 0.85 | 12 | 1.388 | 271.13 ± 0.5 | 270.0 | 395 | 388 | 46.3 ± 1.2 | 43.2 |
3.6 | 0.85 | 11 | 1.369 | 259.02 ± 1.1 | 255.5 | 450 | 489 | 49.7 ± 1.5 | 51.0 |
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Yi, C.; Boluk, Y.; Bindiganavile, V. Experimental Characterization and Multi-Factor Modelling to Achieve Desired Flow, Set and Strength of N-A-S-H Geopolymers. Materials 2022, 15, 5634. https://doi.org/10.3390/ma15165634
Yi C, Boluk Y, Bindiganavile V. Experimental Characterization and Multi-Factor Modelling to Achieve Desired Flow, Set and Strength of N-A-S-H Geopolymers. Materials. 2022; 15(16):5634. https://doi.org/10.3390/ma15165634
Chicago/Turabian StyleYi, Chaofan, Yaman Boluk, and Vivek Bindiganavile. 2022. "Experimental Characterization and Multi-Factor Modelling to Achieve Desired Flow, Set and Strength of N-A-S-H Geopolymers" Materials 15, no. 16: 5634. https://doi.org/10.3390/ma15165634