Mitigating Shrinkage in Superplasticizer-Free Natural Hydraulic Lime Grouts for Historic Masonry Conservation: Effects of Composition, Curing, and Expansion Agents
Abstract
1. Introduction
2. Materials and Method
2.1. Shrinkage Experiment
2.1.1. Raw Materials
2.1.2. Sample Preparation
2.1.3. Curing
2.1.4. Shrinkage Evaluation
2.2. Shrinkage Compensation Test
2.3. Grouting Simulation
3. Results and Discussion
3.1. Forms of Shrinkage Cracks
3.2. Parameters Related to the Shrinkage of Lime Grouts
3.2.1. Type of NHL
3.2.2. Curing Age
3.2.3. Aggregate and Water/Binder Ratio
3.2.4. Curing Condition
3.3. Shrinkage Compensation by Expansive Agent
3.4. Effect of Substrate on Shrinkage
4. Conclusions and Outlook
- (1)
- Shrinkage of lime grouts was mainly affected by aggregate and w/b ratio. When the w/b increased from 0.6 to 0.8, the shrinkage rises by 40%; however, while with the addition of 40% marble powder as an aggregate, the shrinkage reduced by 40%.
- (2)
- The three natural hydraulic limes, NHL2, NHL3.5, and NHL5, showed almost identical in terms of shrinkage properties, but NHL5 has lowest shrinkage performance under same conditions
- (3)
- Under the standard curing conditions (T = 20 ± 2 °C, RH = 65 ± 5%), the shrinkage of NHL grout stabilizes within 14 days, but this time will be delayed to 3 even 5 weeks if the curing environment is hot and humid, or if it was dry and cold.
- (4)
- Magnesium oxide expanders were slow-acting, making it difficult to determine the optimum dosage in a short time; only 0.2% of plastic expanders can lead to significant expansion, making it difficult to control in practice. UEA expanders are also not recommended because they bring soluble salts.
- (5)
- Calcium oxide expansive agent was recommended, with calcium hydroxide as the reaction product, which was the same as that of the lime grout, and the 5–10% dosage was also easy to mix during practical application.
- (6)
- Special attention needs to be paid to the fact that the water absorption of the masonry being repaired will significantly affect the final shrinkage or expansion. For the materials with high water absorption, such as sandstone and old bricks, whose capillary water absorption coefficient exceed 25 kg/m2 h1/2, it is recommended to control shrinkage by optimizing the proportion of grouts rather than using expansive agents. For weakly absorbent substrate materials such as granite or marble, expansive agents should be added appropriately.
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
- Noemi, G.M.; Pablo, M.; Gerardo, G.D.S.; María, D. Historic Masonry; IntechOpen: Rijeka, Croatia, 2019; Chapter 4. [Google Scholar]
- Grimm, C.T. Masonry Cracks: A Review of the Literature. In Masonry: Materials, Design, Construction, and Maintenance; ASTM International: West Conshohocken, PA, USA, 1988. [Google Scholar]
- Wu, Y.; Zhang, B.; Zhang, J.; Zhai, K.; Luo, L. Weathering Characteristics of White Marble Relics Around the Hall of Supreme Harmony (Taihe Dian) in the Forbidden City. KSCE J. Civ. Eng. 2023, 27, 794–804. [Google Scholar] [CrossRef]
- Meng, Q.; Hu, L.; Wan, D.; Li, M.; Wu, H.; Qi, X.; Tian, Y. Image-Based Concrete Cracks Identification Under Complex Background with Lightweight Convolutional Neural Network. KSCE J. Civ. Eng. 2023, 27, 5231–5242. [Google Scholar] [CrossRef]
- Latifi, R.; Hadzima-Nyarko, M.; Radu, D.; Rouhi, R. A Brief Overview On Crack Patterns, Repair and Strengthening of Historical Masonry Structures. Materials 2023, 16, 1882. [Google Scholar] [CrossRef] [PubMed]
- Müller, U.; Miccoli, L.; Fontana, P. Development of a Lime Based Grout for Cracks Repair in Earthen Constructions. Constr. Build. Mater. 2016, 110, 323–332. [Google Scholar] [CrossRef]
- Thotakura, V.N.; Gobinath, R. Strengthening Substrates: Grouting Methods. In Ground Improvement Techniques for Sustainable Engineering; Bentham Science Publishers: Sharjah, United Arab Emirates, 2025. [Google Scholar]
- Carran, D.; Hughes, J.; Leslie, A.; Kennedy, C. A Short History of the Use of Lime as a Building Material Beyond Europe and North America. Int. J. Archit. Herit. 2012, 6, 117–146. [Google Scholar] [CrossRef]
- Christodoulou, D.; Lokkas, P.; Markou, I.; Droudakis, A.; Chouliaras, I.; Alamanis, N. Principles and Developments in Soil Grouting: A Historical Review. Wseas Trans. Adv. Eng. Educ. 2021, 18, 175–191. [Google Scholar] [CrossRef]
- Papayianni, I.; Bicer-Simsir, B.; Jornet, A.; Groot, C.; Valek, J.; Bokan-Bosiljkov, V.; Van Hees, R.; Padovnik, A.; Pachta, V. Rilem Tc 243-Sgm Report: Grouting for Historic Architectural Surfaces. Mater. Struct. 2023, 56, 1. [Google Scholar] [CrossRef]
- Al-Khadaar, R.M.; Ahmed, M.D. Review of Jet Grouting Practice Around the World. J. Eng. 2023, 29, 48–70. [Google Scholar] [CrossRef]
- Silva, B.A.; Pinto, A.F.; Gomes, A. Natural Hydraulic Lime Versus Cement for Blended Lime Mortars for Restoration Works. Constr. Build. Mater. 2015, 94, 346–360. [Google Scholar] [CrossRef]
- Arizzi, A.; Parra-Fernandez, C. A Comprehensive Review of the Manufacturing Process and Properties of Natural Hydraulic Limes. Mater. Struct. 2025, 58, 152. [Google Scholar] [CrossRef]
- Allen, G. Hydraulic Lime Mortar for Stone, Brick and Block Masonry: A Best Practice Guide; Routledge: Donhead St Mary, UK, 2015. [Google Scholar]
- Yue, W.; Wang, B. Ceramic-Added Lime and Cement Mortars: A Review of Applications in Building Products. Sci. Prog. 2024, 107, 00368504241266559. [Google Scholar] [CrossRef]
- Pachta, V.; Chatzineofytou, K. Performance of Brick Masonry Prisms Retrofitted with Fiber Reinforced Lime-Based Grouts. Constr. Build. Mater. 2024, 411, 134370. [Google Scholar] [CrossRef]
- Pachta, V. The Role of Glass Additives in the Properties of Lime-Based Grouts. Heritage 2021, 4, 906–916. [Google Scholar] [CrossRef]
- De La Rosa, Á.; Ruiz, G.; Moreno, R. Analysis of the Rheological Properties of Natural Hydraulic Lime-Based Suspensions for Sustainable Construction and Heritage Conservation. Materials 2024, 17, 825. [Google Scholar] [CrossRef] [PubMed]
- Wei, X.; Chai, Y.; Li, Y.; Wang, W.; Luo, H.; Zhang, B.; Qin, Y. New Discovery of Diethyl Carbonate Modified Natural Hydraulic Lime in Heritage Conservation. Int. J. Archit. Herit. 2024, 1–13. [Google Scholar] [CrossRef]
- Jia, M.; Zhao, Y.; Wu, X.; Ma, X. The Effect of Carbonation Accelerator On Enhancing the Carbonation Process and Mechanical Strength of Air-Hardening Lime Mortars. Constr. Build. Mater. 2024, 425, 136067. [Google Scholar] [CrossRef]
- Pozo-Antonio, J.S. Evolution of Mechanical Properties and Drying Shrinkage in Lime-Based and Lime Cement-Based Mortars with Pure Limestone Aggregate. Constr. Build. Mater. 2015, 77, 472–478. [Google Scholar] [CrossRef]
- Elsen, J.; Van Balen, K.; Mertens, G. Hydraulicity in Historic Lime Mortars: A Review. In Historic Mortars: Characterisation, Assessment and Repair; Springer: Dordrecht, The Netherlands, 2012; pp. 125–139. [Google Scholar]
- Zhang, B.; Zhu, H.; Cheng, Y.; Huseien, G.F.; Shah, K.W. Shrinkage Mechanisms and Shrinkage-Mitigating Strategies of Alkali-Activated Slag Composites: A Critical Review. Constr. Build. Mater. 2022, 318, 125993. [Google Scholar] [CrossRef]
- Zhang, B.; Zhu, H.; Feng, P.; Zhang, P. A Review On Shrinkage-Reducing Methods and Mechanisms of Alkali-Activated/Geopolymer Systems: Effects of Chemical Additives. J. Build. Eng. 2022, 49, 104056. [Google Scholar] [CrossRef]
- Tran, N.P.; Gunasekara, C.; Law, D.W.; Houshyar, S.; Setunge, S.; Cwirzen, A. A Critical Review On Drying Shrinkage Mitigation Strategies in Cement-Based Materials. J. Build. Eng. 2021, 38, 102210. [Google Scholar] [CrossRef]
- Silva, B.; Pinto, A.P.F.; Gomes, A.; Candeias, A. Fresh and Hardened State Behaviour of Aerial Lime Mortars with Superplasticizer. Constr. Build. Mater. 2019, 225, 1127–1139. [Google Scholar] [CrossRef]
- Aghaee, K.; Sposito, R.; Thienel, K.; Khayat, K.H. Effect of Additional Water Or Superplasticizer On Key Characteristics of Cement Paste Made with Superabsorbent Polymer and Other Shrinkage Mitigating Materials. Cem. Concr. Compos. 2023, 136, 104893. [Google Scholar] [CrossRef]
- Yoo, D.; Ryu, G.; Yuan, T.; Koh, K. Mitigating Shrinkage Cracking in Posttensioning Grout Using Shrinkage-Reducing Admixture. Cem. Concr. Compos. 2017, 81, 97–108. [Google Scholar] [CrossRef]
- Baltazar, L.G.; Henriques, F.M.; Jorne, F.; Cidade, M.T. Combined Effect of Superplasticizer, Silica Fume and Temperature in the Performance of Natural Hydraulic Lime Grouts. Constr. Build. Mater. 2014, 50, 584–597. [Google Scholar] [CrossRef]
- Desarnaud, J. Salts in Heritage Sites. In Salt Crystallization in Porous Media; Wiley-ISTE: Hoboken, NJ, USA, 2024; pp. 163–188. [Google Scholar]
- Price, C. Salt Damage in Porous Materials: A Threat to the Cultural Heritage. Archaeol. Int. 2012, 1, 47. [Google Scholar] [CrossRef]
- Pasian, C.; Porter, J.H.; Gorodetska, M.; Parisi, S. Developing a Lime-Based Injection Grout with No Additives for Very Thin Delamination: The Role of Aggregates and Particle Size/Morphology; Springer: Cham, Switzerland, 2022. [Google Scholar]
- Bras, A.; Henriques, F.M.A. The Influence of the Mixing Procedures On the Optimization of Fresh Grout Properties. Mater. Struct. 2009, 42, 1423–1432. [Google Scholar] [CrossRef]
- Grilo, J.; Faria, P.; Veiga, R. New Natural Hydraulic Lime Mortars—Physical and Microstructural Properties in Different Curing Conditions. Constr. Build. Mater. 2014, 54, 378–384. [Google Scholar] [CrossRef]
- JGJ/T 70-2009; Ministry of Housing and Urban-Rural Development of the People’s Republic of China. Standard for Test Method of Performance on Building Mortar. China Building Industry Press: Beijing, China, 2009.
- WW/T 0063-2015; Code for Investigation of the Protection Engineering of the Stone Monument. National Cultural Heritage Administration: Beijing, China, 2015.
- Chi, Y.Y. Effect of Expansion Agent On Properties of Cement-Based Grout. Master’s Thesis, Chang’an University, Xi’an, China, 2022. [Google Scholar]
- Xu, Y.; Zhang, H.; Yu, X.; Qian, Y. Development and Evaluation of Physical and Mechanical Properties of Alkali-Activated Multi-Component Composite Grouting Materials. Constr. Build. Mater. 2024, 434, 136718. [Google Scholar] [CrossRef]
- Zhang, G.; Qiu, D.; Wang, S.; Wang, P. Effects of Plastic Expansive Agent On the Fluidity, Mechanical Strength, Dimensional Stability and Hydration of High Performance Cementitious Grouts. Constr. Build. Mater. 2020, 243, 118204. [Google Scholar] [CrossRef]
- Sisomphon, K.; Copuroglu, O.; Koenders, E. Self-Healing of Surface Cracks in Mortars with Expansive Additive and Crystalline Additive. Cem. Concr. Compos. 2012, 34, 566–574. [Google Scholar] [CrossRef]
Materials | Oxides Composition (wt%) | Apparent Density (g/cm3) | Surface Color | ||||
---|---|---|---|---|---|---|---|
Al2O3 | Fe2O3 | SiO2 | CaO | MgO | |||
NHL2 | 1.10 | 0.55 | 11.20 | 62.60 | 1.44 | 2.21 | ash gray |
NHL3.5 | 1.59 | 0.58 | 18.89 | 55.95 | 1.90 | 2.29 | ash gray |
NHL5 | 1.62 | 0.58 | 19.98 | 55.60 | 1.02 | 2.46 | ash gray |
Marble powder | 6.53 | 0.29 | 4.85 | 80.61 | 0.06 | 2.72 | matte white |
Factors | |||
---|---|---|---|
A (Marble Powder) | B (Water/Binder Ratio) | C (Curing Condition) | |
1 | 1 (0%) | 1 (0.6) | 1 (C1 = 10 °C, 35% RH) |
2 | 1 (0%) | 2 (0.7) | 3 (C3 = 30 °C, 95% RH) |
3 | 1 (0%) | 3 (0.8) | 2 (C2 = 20 °C, 65% RH) |
4 | 2 (20%) | 1 (0.6) | 3 (C3 = 30 °C, 95% RH) |
5 | 2 (20%) | 2 (0.7) | 2 (C2 = 20 °C, 65% RH) |
6 | 2 (20%) | 3 (0.8) | 1 (C1 = 10 °C, 35% RH) |
7 | 3 (40%) | 1 (0.6) | 2 (C2 = 20 °C, 65% RH) |
8 | 3 (40%) | 2 (0.7) | 1 (C1 = 10 °C, 35% RH) |
9 | 3 (40%) | 3 (0.8) | 3 (C3 = 30 °C, 95% RH) |
Main Content (%) | Specific Surface Area (m2/kg) | Surface Color | |||||
---|---|---|---|---|---|---|---|
CaO | MgO | SiO2 | Fe2O3 | Al2O3 | |||
EA-Ca | 74.5 | 4.3 | 3.3 | 3.1 | 2.5 | 345 | dark gray |
EA-Mg | 3.5 | 82.5 | 6.3 | 0.7 | 0.9 | 320 | light brown |
EA-u | 11.3 | 2.5 | 40.1 | 4.7 | 14.9 | 270 | white |
EA-p | 27.5 | 22.5 | 14.5 | 13.2 | 3.4 | 315 | faint yellow |
Substrate Material | Total Porosity (%) | Capillary Water Absorption Coefficient (kg/m2 h1/2) |
---|---|---|
Sandstone | 12.20 | 8.40 |
Green clay brick | 28.90 | 18.70 |
White marble | 0.56 | 0.08 |
Plastic board | 0.00 | 0.00 |
Factor | Result | |||
---|---|---|---|---|
A | B | C | Shrinkage (%) | |
1 | 1(0) | 1(0.6) | 1(C1) | 1.62 |
2 | 1 | 2(0.7) | 2(C2) | 1.88 |
3 | 1 | 3(0.8) | 3(C3) | 2.11 |
4 | 2(20) | 1 | 3 | 1.34 |
5 | 2 | 2 | 2 | 1.53 |
6 | 2 | 3 | 1 | 1.74 |
7 | 3(40) | 1 | 2 | 0.79 |
8 | 3 | 2 | 1 | 0.95 |
9 | 3 | 3 | 3 | 1.30 |
K1 | 5.61 | 3.75 | 4.31 | Σ = 13.26 |
K2 | 4.61 | 4.36 | 4.2 | |
K3 | 3.04 | 5.15 | 4.75 | |
1.87 | 1.25 | 1.44 | ||
1.54 | 1.45 | 1.40 | ||
1.01 | 1.72 | 1.58 | ||
Excellent level | A3 | B1 | C2 | |
R | 0.86 | 0.26 | 0.18 |
Disclaimer/Publisher’s Note: The statements, opinions and data contained in all publications are solely those of the individual author(s) and contributor(s) and not of MDPI and/or the editor(s). MDPI and/or the editor(s) disclaim responsibility for any injury to people or property resulting from any ideas, methods, instructions or products referred to in the content. |
© 2025 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.org/licenses/by/4.0/).
Share and Cite
Wu, Y.; Dai, S. Mitigating Shrinkage in Superplasticizer-Free Natural Hydraulic Lime Grouts for Historic Masonry Conservation: Effects of Composition, Curing, and Expansion Agents. Materials 2025, 18, 3791. https://doi.org/10.3390/ma18163791
Wu Y, Dai S. Mitigating Shrinkage in Superplasticizer-Free Natural Hydraulic Lime Grouts for Historic Masonry Conservation: Effects of Composition, Curing, and Expansion Agents. Materials. 2025; 18(16):3791. https://doi.org/10.3390/ma18163791
Chicago/Turabian StyleWu, Yang, and Shibing Dai. 2025. "Mitigating Shrinkage in Superplasticizer-Free Natural Hydraulic Lime Grouts for Historic Masonry Conservation: Effects of Composition, Curing, and Expansion Agents" Materials 18, no. 16: 3791. https://doi.org/10.3390/ma18163791
APA StyleWu, Y., & Dai, S. (2025). Mitigating Shrinkage in Superplasticizer-Free Natural Hydraulic Lime Grouts for Historic Masonry Conservation: Effects of Composition, Curing, and Expansion Agents. Materials, 18(16), 3791. https://doi.org/10.3390/ma18163791