The Effect of Exposure on the Autogenous Self-Healing of Ordinary Portland Cement Mortars
Abstract
:1. Introduction
2. Materials and Methods
3. Results
3.1. Crack Closure Ratio, pH Changes and Self-Healing Products
3.1.1. Water Immersion Regime
3.1.2. Temperature
3.1.3. Accelerating and Retarding Admixtures
3.1.4. Calcium Ions and Silica Microparticles
3.2. Strength Recovery
4. Discussion
5. Conclusions
- The water-related exposures did not give satisfying self-healing results despite the application of different cycles or water volumes. A higher ion concentration, expected in the case of a smaller amount of water present inside of the crack, did not support the healing process;
- The addition of the phosphate-based retarding admixture demonstrated the highest crack closure both internally and externally. Phosphate ions were found to contribute to the filling of the crack, most likely by preventing the formation of a dense shell composed of the hydration phases on the exposed crack by unhydrated cement grains. Phosphate ions also caused the formation of calcium–phosphate based compounds;
- The highest strength recovery and a very good crack closure ratio was achieved by immersion in water mixed with microsilica particles. The micro sized silica particles presumably served as nucleation sites for the formation of the CSH, calcium carbonate, and Portlandite.
- The applied chemicals were of an industrial/technical grade, which generated a number of different factors that should be considered. Even though this is the case in real-life concrete applications, in order to fully understand the mechanisms of the autogenous self-healing, higher purity chemical substances should be used to separate the variables;
- The SEM evaluation should be performed on a larger number of specimens in order to enable quantitative evaluation of the internal self-healing products. It is especially crucial due to the strong effects of the crack width and shape;
- In order to fully confirm the chemical composition of the precipitated self-healing phases, the performed elemental analysis should be complemented by an evaluation of the mineralogical composition using, for example an X-ray powder diffraction (XRD). Larger specimens should be tested, thus increasing the amount of the analyzed phases;
- As the used retarding admixture significantly enhanced the self-healing efficiency, different kinds of retarders could be compared;
- Mineralogical composition, solubility, durability, and other physical properties of the calcium phosphate phase should be verified with respect to its full scale applicability;
- The combination of different exposures, which showed the highest self-healing efficiency, could be tested, e.g., a retarding admixture together with microsilica particles.
Author Contributions
Funding
Conflicts of Interest
References
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Chemical Analysis | Mean Value (%) |
---|---|
CaO | 63.30 |
SiO2 | 21.20 |
Al2O3 | 3.40 |
Fe2O3 | 4.10 |
MgO | 2.20 |
Na2O | 0.18 |
K2O | 0.56 |
SO3 | 2.70 |
Cl | <0.01 |
Loss of ignition | 2.50 |
Water soluble Cr6+ | <2 mg/kg |
Na2O-eq. | 0.55 |
Exposure | Abbreviation | Justification |
---|---|---|
Air | EXP 0 | Non-healed samples |
Deionized water mixed with Accelerator in proportions 3:1 (immersion) | EXP 1 | Increasing the rate of hydration process inside the crack; possibly faster healing; different composition of hydrates [26,27,28] |
Deionized water mixed with Retarder in proportions 3:1 (immersion) | EXP 2 | Slowing down the hydration—more hydrates can precipitate on the surface of unhydrated cement grains [27,29] |
Saturated lime water immersion | EXP 3 | More Ca2+ ions in the solution, higher pH |
Deionized water immersion | EXP 4 | Reference exposure |
Deionized water immersion with cyclic evaporation (72 h cycle) | EXP 5 | Changing of the water regime by introducing the cycles of evaporation as well as different volume of water in order to modify the concentration of ions inside the crack |
Dry/wet (deionized water) cycles; 24 h dry and 24 h immersion in water | EXP 6 | |
Deionized water immersion up to 1 mm height of the sample | EXP 7 | |
Deionized water immersion up to 5 mm height of the sample | EXP 8 | |
Water immersion temperature cycle 24 h/20 °C and 24 h/40 °C | EXP 9 | Increasing/decreasing the rate of the hydration process as well changing the hydration products composition. Possible ettringite formation leading to a higher strength regain in case of lower temperature [30,31] |
Water immersion temperature cycle 24 h/20 °C and 24 h/5 °C | EXP 10 | |
Deionized immersion with microsilica particles 1.25 %w | EXP 11 | Providing the nucleation sites inside the crack for the self-healing products |
Phase | Composition | Ca/P |
---|---|---|
Brushite (DCPD) | CaHPO4 2H2O | 1.00 |
Monetite (DCPA) | CaHPO4 | 1.00 |
Octacalcium phosphate (OCP) | Ca4H(PO4)3 2.5H2O | 1.33 |
Whitlockite/tricalcium phosphate (TCP) | Ca3H(PO4)2 | 1.50 |
Hydroxyapatite (HAP) | Ca5(PO4)3OH | 1.67 |
Amorphous calcium phosphate (ACP) | - | - |
Exposure | Abbreviation | External Self-Healing | Internal Self-Healing |
---|---|---|---|
Deionized water mixed with Accelerator in proportions 3:1 (immersion) | EXP 1 | Very limited crack closure; Several calcite crystals of various shapes | Almost no healing; Several microns thick calcite layer under the surface, inside—few thicker deposits of calcite mixed with CSH (Si/Ca = 0.19) |
Deionized water mixed with Retarder in proportions 3:1 (immersion) | EXP 2 | The crack almost completely healed; calcium phosphate compounds on the surface with some amount of sodium originating from the self-healing mixture | Very high internal crack closure; Calcium phosphate compounds as well as CSH; Si/Ca and Ca/P increasing with crack depth |
Saturated lime water immersion | EXP 3 | Very good external self-healing; dense layer of calcite crystals present at the surface | Almost no internal self-healing; few self-healing products with average Si/Ca of 0.3 |
Deionized water immersion | EXP 4 | Very limited external healing, ettringite and calcite crystals filling the crack | Ettringite visible close to the surface; no internal self-healing |
Deionized water immersion with cyclic evaporation (72 h cycle) | EXP 5 | Some crack closure; bigger calcite crystals covering the crack | Layer of calcite inside of the sample closure to the surface, few self-healing products in deeper parts of the crack |
Dry/wet (deionized water) cycles 24 h/24 h | EXP 6 | Almost no external self-healing with small calcite crystal layer at the surface | No internal self-healing except for few healing products deposited on the PVA fibers surface |
Deionized water immersion up to 1 mm height of the sample | EXP 7 | Minimal external healing, ettringite present; no noticeable differences between exposure 8 and 9 | Ettringite visible close to the surface; no internal self-healing |
Deionized water immersion up to 5 mm height of the sample | EXP 8 | ||
Water immersion temperature cycle 24 h/20 °C and 24 h/40 °C | EXP 9 | Very limited external healing, calcite crystals filling the crack | Hardly any internal healing with only single calcite crystals |
Water immersion temperature cycle 24 h/20 °C and 24 h/5 °C | EXP 10 | Efficient external crack closing; calcite crystals inside the crack as well as thick layer of ettringite | |
Deionized immersion with microsilica particles 1.25%w | EXP 11 | Very high external self-healing with densified calcite structure filling the crack | Agglomerates of microsilica particles inside the crack without self-healing products. |
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Rajczakowska, M.; Habermehl-Cwirzen, K.; Hedlund, H.; Cwirzen, A. The Effect of Exposure on the Autogenous Self-Healing of Ordinary Portland Cement Mortars. Materials 2019, 12, 3926. https://doi.org/10.3390/ma12233926
Rajczakowska M, Habermehl-Cwirzen K, Hedlund H, Cwirzen A. The Effect of Exposure on the Autogenous Self-Healing of Ordinary Portland Cement Mortars. Materials. 2019; 12(23):3926. https://doi.org/10.3390/ma12233926
Chicago/Turabian StyleRajczakowska, Magdalena, Karin Habermehl-Cwirzen, Hans Hedlund, and Andrzej Cwirzen. 2019. "The Effect of Exposure on the Autogenous Self-Healing of Ordinary Portland Cement Mortars" Materials 12, no. 23: 3926. https://doi.org/10.3390/ma12233926