Performance Recovery of Phase Change Materials (PCMs)-Modified Limestone Calcined Clay Cement (LC3) Composite Through Air-Void Control Using a Silicone-Based Defoamer
DOI:
https://doi.org/10.12974/2311-8717.2026.14.01Keywords:
Limestone calcined clay cement (LC3), Phase change materials (PCMs), Defoamer, Capric acidAbstract
Limestone calcined clay cement (LC3) has emerged as a promising low-carbon alternative to ordinary Portland cement (OPC) due to its reduced clinker content and associated carbon footprint. In parallel, integrating phase change materials (PCMs) into cementitious composites offers a pathway to enhance building thermal regulation through latent heat storage. However, hydrophobic PCMs may adversely affect fresh workability and hardened performance, particularly by promoting entrapped air and increasing porosity. This study investigates the incorporation of capric acid (CA) as an organic PCMs through partial cement replacement (0%, 1%, 5%, and 10% by mass) in OPC and LC3 mortars. In this context, the mortar is a functional organic–inorganic composite, where the organic PCMs phase contributes thermal energy storage functionality. Unlike most PCMs studies focused on OPC systems, this work emphasises LC3 and identifies air-void control as a critical mechanism for performance recovery in LC3–PCMs composites. It also evaluates the effectiveness of a silicone-based defoamer (0.15% by mass of the total mixture) in mitigating air-related performance losses. Fresh flowability, hardened density, ultrasonic pulse velocity, and compressive strength were determined up to 28 days. Results showed that increasing CA content reduced flowability, density, UPV, and compressive strength in both OPC and LC3 systems, indicating that hydrophobic PCMs inclusion adversely affected matrix continuity. However, the incorporation of a silicone-based defoamer enabled performance recovery in both OPC and LC3 composites by improving matrix compactness through air-void control. Overall, the results demonstrate that air-void control is critical for PCMs-modified mortars, and that defoamer addition provides a practical approach to improve the performance of LC3–PCMs systems while maintaining their sustainability benefits.
References
S. Sbahieh, G. McKay, A. Nurdiawati, S.G. Al-Ghamdi, The sustainability of partial and total replacement of Ordinary Portland Cement: A deep dive into different concrete mixtures through life cycle assessment, Journal of Building Engineering 108 (2025) 112830. https://doi.org/10.1016/j.jobe.2025.112830
F. Belaïd, How does concrete and cement industry transformation contribute to mitigating climate change challenges?, Resources, Conservation & Recycling Advances 15 (2022) 200084. https://doi.org/10.1016/j.rcradv.2022.200084
Y.T. Chan, N.H.A.S. Lim, S. Ishak, M. Samadi, S.P. Ngian, H.Y. Kek, S.Q. Tan, Mechanical and Microstructural Performances of One-Part Alkali-Activated Fly Ash Mortars with Thermally Activated Palm Oil Decanter Cake, Journal of Composites and Biodegradable Polymers 13 (2025) 183-201. https://doi.org/10.12974/2311-8717.2025.13.16
Y.T. Chan, N.H. Abdul Shukor Lim, S.A. Abd Latif, S. Ishak, P.S. Lee, S.Q. Tan, A. Azhar, J.J. Moy, H.Y. Kek, Scientometric Review of One-Part Geopolymer Composites, International Conference on Intelligent Information Technologies, Springer, 2018, pp. 407-416. https://doi.org/10.1007/978-981-96-3804-8_36
B. Lothenbach, K. Scrivener, R.D. Hooton, Supplementary cementitious materials, Cement and Concrete Research 41(12) (2011) 1244-1256. https://doi.org/10.1016/j.cemconres.2010.12.001
Y.-S. Wang, S. Oh, S. Ishak, X.-Y. Wang, S. Lim, Recycled glass powder for enhanced sustainability of limestone calcined clay cement (LC3) mixtures: mechanical properties, hydration, and microstructural analysis, Journal of Materials Research and Technology 27 (2023) 4012-4022. https://doi.org/10.1016/j.jmrt.2023.10.245
K. Hosen, B. Chen, Limestone calcined clay cement (LC3): A review of materials, properties, production and environmental impact, Journal of Building Engineering 112 (2025) 113672. https://doi.org/10.1016/j.jobe.2025.113672
K. Scrivener, F. Martirena, S. Bishnoi, S. Maity, Calcined clay limestone cements (LC3), Cement and Concrete Research 114 (2018) 49-56. https://doi.org/10.1016/j.cemconres.2017.08.017
J. Sun, F. Zunino, K. Scrivener, Hydration and phase assemblage of limestone calcined clay cements (LC3) with clinker content below 50 %, Cement and Concrete Research 177 (2024) 107417. https://doi.org/10.1016/j.cemconres.2023.107417
F.S. Hafez, B. Sa'di, M. Safa-Gamal, Y.H. Taufiq-Yap, M. Alrifaey, M. Seyedmahmoudian, A. Stojcevski, B. Horan, S. Mekhilef, Energy Efficiency in Sustainable Buildings: A Systematic Review with Taxonomy, Challenges, Motivations, Methodological Aspects, Recommendations, and Pathways for Future Research, Energy Strategy Reviews 45 (2023) 101013. https://doi.org/10.1016/j.esr.2022.101013
S. Ishak, M. Yio, J. Moon, S. Mandal, S. Sasui, N.H. Abdul Shukor Lim, X.-Y. Wang, Y.-S. Wang, M.M. Al Bakri Abdullah, P.N. Shek, Hydration and microstructural development of cement pastes incorporating diatomaceous earth, expanded perlite, and shape-stabilized phase change materials (SSPCMs), Construction and Building Materials 468 (2025) 140483. https://doi.org/10.1016/j.conbuildmat.2025.140483
S. Ishak, S. Mandal, H.-S. Lee, D.-E. Lee, Z. Chen, Structure-property correlation of thermally activated nano-size phase change material in the cementitious system, Journal of Building Engineering 66 (2023) 105871. https://doi.org/10.1016/j.jobe.2023.105871
S. Mandal, A.C. Mendhe, Y.N. Singhbabu, H.-S. Lee, T. Park, S. Ishak, Physical, chemical, and thermal properties of porous expanded perlite-based phase change composite and their effects on the hydration kinetics, Case Studies in Construction Materials 22 (2025) e04510. https://doi.org/10.1016/j.cscm.2025.e04510
S. Ishak, H. Lgaz, S. Mandal, R.J. Adnin, D.-E. Lee, H.-S. Lee, N.S. Mohammad Harmay, M.M. Al Bakri Abdullah, X.-Y. Wang, H.-M. Yang, Multi-technique investigation on the surface interaction of diatomaceous earth with organic phase change material: Experimental and molecular dynamics aspects, Journal of Molecular Liquids 391 (2023) 123292. https://doi.org/10.1016/j.molliq.2023.123292
Ł. Mika, E. Radomska, K. Sztekler, A. Gołdasz, W. Zima, Review of Selected PCMs and Their Applications in the Industry and Energy Sector, Energies, 2025, p. 1233. https://doi.org/10.3390/en18051233
A. Anand, M. Mansor, K. Sharma, A. Shukla, A. Sharma, M.I.H. Siddiqui, K.K. Sadasivuni, N. Priyadarshi, B. Twala, A comprehensive review on eutectic phase change materials: Development, thermophysical properties, thermal stability, reliability, and applications, Alexandria Engineering Journal 112 (2025) 254-280. https://doi.org/10.1016/j.aej.2024.10.054
R. Baetens, B.P. Jelle, A. Gustavsen, Phase change materials for building applications: A state-of-the-art review, Energy and Buildings 42(9) (2010) 1361-1368. https://doi.org/10.1016/j.enbuild.2010.03.026
S. Ishak, S. Mandal, H. Lgaz, D.G. Atinafu, N.S. Mohammad Harmay, H.-S. Lee, N. Abdul Shukor Lim, M.M.A.B. Abdullah, H.-M. Yang, Microscopic molecular insights of different carbon chain fatty acids on shape-stabilized phase change composite, Journal of Thermal Analysis and Calorimetry 149(17) (2024) 9203-9221. https://doi.org/10.1007/s10973-024-13539-0
G. Hekimoğlu, M. Nas, M. Ouikhalfan, A. Sarı, V.V. Tyagi, R.K. Sharma, Ş. Kurbetci, T.A. Saleh, Silica fume/capric acid-stearic acid PCM included-cementitious composite for thermal controlling of buildings: Thermal energy storage and mechanical properties, Energy 219 (2021) 119588. https://doi.org/10.1016/j.energy.2020.119588
F. Meng, L. Dong, Y. Wu, X. Shu, Y. Guo, Q. Ran, Effects and mechanisms of capric acid/silica capsule on water absorption reduction of cement paste, Construction and Building Materials 404 (2023) 133208. https://doi.org/10.1016/j.conbuildmat.2023.133208
S. Drissi, T.-C. Ling, K.H. Mo, A. Eddhahak, A review of microencapsulated and composite phase change materials: Alteration of strength and thermal properties of cement-based materials, Renewable and Sustainable Energy Reviews 110 (2019) 467-484. https://doi.org/10.1016/j.rser.2019.04.072
M.M. Alsaadawi, M. Amin, A.M. Tahwia, Thermal, mechanical and microstructural properties of sustainable concrete incorporating Phase change materials, Construction and Building Materials 356 (2022) 129300. https://doi.org/10.1016/j.conbuildmat.2022.129300
M. Qiao, J. Wu, N. Gao, G. Shan, F. Shen, J. Chen, B. Zhu, Preparation and Properties of Different Polyether-Type Defoamers for Concrete, Materials, 2022, p. 7492. https://doi.org/10.3390/ma15217492
J. Hu, Y. Xie, Z. Liu, Z. Weng, Y. Wang, K. Li, Effectiveness of air entraining agent and defoamer on the bubble distribution of fresh mortar under different mixing methods, IOP Conference Series: Earth and Environmental Science 371(4) (2019) 042012. https://doi.org/10.1088/1755-1315/371/4/042012
L. Yuan, Y. Ma, J. Zhang, J. Men, T. Sun, H. Zhao, H. Wu, H. Wang, S. Dai, Orthogonal analysis and mechanism of compressive strength and microstructure of the metakaolin-fly ash geopolymer, Case Studies in Construction Materials 17 (2022) e01154. https://doi.org/10.1016/j.cscm.2022.e01154
F. Zunino, K. Scrivener, The reaction between metakaolin and limestone and its effect in porosity refinement and mechanical properties, Cement and Concrete Research 140 (2021) 106307. https://doi.org/10.1016/j.cemconres.2020.106307
ASTM C1437, Standard Test Method for Flow of Hydraulic Cement Mortar, ASTM International, West Conshohocken, 2020, p. 2.
ASTM C642, Standard Test Method for Density, Absorption, and Voids in Hardened Concrete, ASTM International, West Conshohocken, 2021, p. 3.
ASTM C597, Standard Test Method for Ultrasonic Pulse Velocity Through Concrete, ASTM International, West Conshohocken, 2022, p. 4.
ASTM C109, Standard Test Method for Compressive Strength of Hydraulic Cement Mortars (Using 2-in. or [50-mm] Cube Specimens), ASTM International, West Conshohocken, 2022, p. 11.
S. Cunha, M. Lima, J.B. Aguiar, Influence of adding phase change materials on the physical and mechanical properties of cement mortars, Construction and Building Materials 127 (2016) 1-10. https://doi.org/10.1016/j.conbuildmat.2016.09.119
J.L. Trenzado, C. Benito, M. Atilhan, S. Aparicio, Hydrophobic Deep eutectic Solvents based on cineole and organic acids, Journal of Molecular Liquids 377 (2023) 121322. https://doi.org/10.1016/j.molliq.2023.121322
A. Figueiredo, J. Lapa, R. Vicente, C. Cardoso, Mechanical and thermal characterization of concrete with incorporation of microencapsulated PCM for applications in thermally activated slabs, Construction and Building Materials 112 (2016) 639-647. https://doi.org/10.1016/j.conbuildmat.2016.02.225
M. Łach, K. Pławecka, A. Bąk, M. Adamczyk, P. Bazan, B. Kozub, K. Korniejenko, W.-T. Lin, Review of Solutions for the Use of Phase Change Materials in Geopolymers, Materials, 2021, p. 6044. https://doi.org/10.3390/ma14206044
K. Yu, M. Jia, W. Tian, Y. Yang, Y. Liu, Enhanced thermo-mechanical properties of cementitious composites via red mud-based microencapsulated phase change material: Towards energy conservation in building, Energy 290 (2024) 130301. https://doi.org/10.1016/j.energy.2024.130301
L. Ferrari, V. Bortolotti, N. Mikanovic, M. Ben-Haha, E. Franzoni, Influence of calcined clay on workability of mortars with low-carbon cement, Nanoworld Journal 9(Special Issue 2) (2023) S30-S34. https://doi.org/10.17756/nwj.2023-s2-006
H. Zhang, S. Mu, J. Cai, R. Chen, The impact of carboxylic acid type hydrophobic agent on compressive strength of cementitious materials, Construction and Building Materials 291 (2021) 123315. https://doi.org/10.1016/j.conbuildmat.2021.123315
R. Abousnina, F. Aljuaydi, B. Benabed, M.H. Almabrok, V. Vimonsatit, A State-of-the-Art Review on the Influence of Porosity on the Compressive Strength of Porous Concrete for Infrastructure Applications, Buildings 15(13) (2025) 2311. https://doi.org/10.3390/buildings15132311