Abstract
Investigation of the multiscale structural development of cementitious materials plays an essential role in understanding their drying behavior. Portland cement pastes with a fatty-alcohol-based shrinkage reducing agent (SRA) under practical hydration and evaporation conditions were used instead of ultimate states, which have already been reported. The results of small-angle X-ray scattering (SAXS) analysis showed that fractal disc-shaped agglomeration units of the calcium silicate hydrate (C-S-H) increased in size with the addition of the SRA. Water vapor sorption isotherms (WVSI) revealed that mesopores were formed between and/or within the agglomeration units of C-S-H, and the volume of mesopores increased with increasing SRA content. The agglomeration units containing mesopores were stable and reduced the drying shrinkage. This explanation may be extended to the macroscale structure, which predominantly contributes to drying shrinkage at very early ages. In addition, the first reported results of WVSI at extremely low relative pressures and SAXS indicated that the pore structure at the atomic level was not affected by the presence of the SRA.
Similar content being viewed by others
References
Powers TC (1968) Mechanism of shrinkage and reversible creep of hardened cement paste. In: Proceeding of international conference the structure of concrete and its behavior under Load Cement and Concrete Association, London, UK, pp 345–364
Gartner E, Maruyama I, Chen J (2017) A new model for the C-S-H phase formed during the hydration of Portland cements. Cem Concr Res 97:95–106. https://doi.org/10.1016/j.cemconres.2017.03.001
Maruyama I, Sakamoto N, Matsui K, Igarashi G (2017) Microstructural changes in white Portland cement paste under the first drying process evaluated by WAXS, SAXS, and USAXS. Cem Concr Res 91:24–32. https://doi.org/10.1016/j.cemconres.2016.10.002
Maruyama I, Ohkubo T, Haji T, Kurihara R (2019) Dynamic microstructural evolution of hardened cement paste during first drying monitored by 1H NMR relaxometry. Cem Concr Res 122:107–117. https://doi.org/10.1016/j.cemconres.2019.04.017
McDonald PJ, Istok O, Janota M, Gajewicz-Jaromin AM, Faux DA (2020) Sorption, anomalous water transport and dynamic porosity in cement paste: a spatially localised 1H NMR relaxation study and a proposed mechanism. Cem Concr Res 133:106045. https://doi.org/10.1016/j.cemconres.2020.106045
Maruyama I, Beppu K, Kurihara R, Furuta A (2016) Action mechanisms of shrinkage reducing admixture in hardened cement paste. J Adv Concr Technol 14(6):311–323. https://doi.org/10.3151/jact.14.311
Maruyama I, Gartner E, Beppu K, Kurihara R (2018) Role of alcohol-ethylene oxide polymers on the reduction of shrinkage of cement paste. Cem Concr Res 111:157–168. https://doi.org/10.1016/j.cemconres.2018.05.017
Weiss J, Lura P, Rajabipour F, Sant G (2008) Performance of shrinkage reducing admixtures at different humidities and at early ages. ACI Mater J 105:478–486
Saliba J, Rozière E, Grondin F, Loukili A (2011) Influence of shrinkage-reducing admixtures on plastic and long-term shrinkage. Cem Concr Compos 33(2):209–217. https://doi.org/10.1016/j.cemconcomp.2010.10.006
Lura P, Pease B, Mazzotta GB, Rajabipour F, Weiss J (2007) Influence of shrinkage-reducing admixtures on development of plastic shrinkage cracks. ACI Mater J 104-M22:187–194
Maruyama I, Igarashi G, Matsui K, Sakamoto N (2021) Hinderance of C-S-H sheet piling during first drying using a shrinkage reducing agent: a SAXS study. Cem Concr Res 144:106429. https://doi.org/10.1016/j.cemconres.2021.106429
de Burgh JM, Foster SJ (2017) Influence of temperature on water vapour sorption isotherms and kinetics of hardened cement paste and concrete. Cem Concr Res 92:37–55. https://doi.org/10.1016/j.cemconres.2016.11.006
Maruyama I, Nishioka Y, Igarashi G, Matsui K (2014) Microstructural and bulk property changes in hardened cement paste during the first drying process. Cem Concr Res 58:20–34. https://doi.org/10.1016/j.cemconres.2014.01.007
Takahashi K, Asamoto S, Kobayashi M, Bier T (2019) Effects of fatty alcohol-based shrinkage reducing agents on early-age shrinkage under high temperature conditions. J Adv Concr Technol 17(11):648–658. https://doi.org/10.3151/jact.17.648
Tim C (2014) Challenges and opportunities in tropical concreting. Procedia Eng 95:348–355. https://doi.org/10.1016/j.proeng.2014.12.193
Aili A, Maruyama I (2020) Review of several experimental methods for characterization of micro- and nano-scale pores in cement-based material. Int J Concr Struct Mater 14(1):55. https://doi.org/10.1186/s40069-020-00431-y
International Union of Pure and Applied Chemistry, Manual of symbols and terminology (1972) Pure Appl Chem Vol. 31:1, Coll Surf Chem 578–621, Appendix 2
Diamond S (2000) Mercury porosimetry: an inappropriate method for the measurement of pore size distributions in cement-based materials. Cem Concr Res 30(10):1517–1525. https://doi.org/10.1016/S0008-8846(00)00370-7
Brunauer S, Emmett PH, Teller E (1938) Adsorption of gases in multimolecular layers. J Am Ceram Soc 60:309–319
Odler I (2003) The BET-specific surface area of hydrated Portland cement and related materials. Cem Concr Res 33(12):2049–2056. https://doi.org/10.1016/S0008-8846(03)00225-4
Dollimore D, Heal GR (1964) An improved method for the calculation of pore size distribution from adsorption data. J Appl Chem 14(3):109–114. https://doi.org/10.1002/jctb.5010140302
Thommes M (2004) Physical adsorption characterization of ordered and amorphous mesoporous materials. Nanoporous materials: science and engineering, pp 317–364
Naono H, Hakuman M, Tanaka T, Tamura N, Nakai K (2000) Porous texture and surface character of dehydroxylated and rehydroxylated MCM-41 mesoporous silicas–analysis of adsorption isotherms of nitrogen gas and water vapor. J Coll Interf Sci 225(2):411–420. https://doi.org/10.1006/jcis.2000.6777
Thommes M, Kaneko K, Neimark AV, Olivier JP, Rodriguez-Reinoso F, Rouquerol J, Sing KSW (2015) Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC Technical Report) [IUPAC technical report]. Pure Appl Chem 87(9–10):1051–1069. https://doi.org/10.1515/pac-2014-1117
Maruyama I, Rymeš J, Vandamme M, Coasne B (2018) Cavitation of water in hardened cement paste under short-term desorption measurements. Mater Struct 51(6):159. https://doi.org/10.1617/s11527-018-1285-x
Naono H, Hakuman M (1993) Analysis of porous texture by means of water vapor adsorption isotherm with particular attention to lower limit of hysteresis loop. J Coll Interf Sci 158(1):19–26. https://doi.org/10.1006/jcis.1993.1223
Badmann R, Stockhausen N, Setzer M (1981) The statistical thickness and the chemical potential of adsorbed water films. J Colloid Interface Sci 82(2):534–542. https://doi.org/10.1016/0021-9797(81)90395-7
Thommes M, Morell J, Cychosz KA, Fröba M (2013) Combining nitrogen, argon, and water adsorption for advanced characterization of ordered mesoporous carbons (CMKs) and periodic mesoporous organosilicas (PMOs). Langmuir 29(48):14893–14902. https://doi.org/10.1021/la402832b
Winslow DN, Diamond S (1974) Specific surface of hardened Portland cement paste as determined by small-angle X-ray scattering. J Am Ceram Soc 57(5):193–197. https://doi.org/10.1111/j.1151-2916.1974.tb10856.x
Chiang WS, Fratini E, Ridi F, Lim SH, Yeh YQ, Baglioni P, Choi SM, Jeng US, Chen SH (2013) Microstructural changes of globules in calcium-silicate-hydrate gels with and without additives determined by small-angle neutron and X-ray scattering. J Colloid Interf Sci 398:67–73. https://doi.org/10.1016/j.jcis.2013.01.065
Aligizaki KK (2006) Pore structure of cement-based materials. Taylor & Francis, New York, pp 247–285
Allen AJ, Thomas JJ, Jennings HM (2007) Composition and density of nanoscale calcium-silicate-hydrate in cement. Nat Mater 6(4):311–316. https://doi.org/10.1038/nmat1871
Thomas JJ, Allen AJ, Jennings HM (2008) Structural changes to the calcium-silicate-hydrate gel phase of hydrated cement with age, drying, and resaturation. J Am Ceram Soc 91(10):3362–3369. https://doi.org/10.1111/j.1551-2916.2008.02636.x
Nicoleau L, Gädt T, Chitu L, Maier G, Paris O (2013) Oriented aggregation of calcium silicate hydrate platelets by the use of comb-like copolymers. Soft Matter 9(19):4864–4874. https://doi.org/10.1039/c3sm00022b
Guinier A, Fournet G (1955) Small angle scattering of X-rays. Wiley, New York
Richardson IG (1999) The nature of C-S-H in hardened cements. Cem Concr Res 29(8):1131–1147. https://doi.org/10.1016/S0008-8846(99)00168-4
Jennings HM (2000) A model for the microstructure of calcium silicate hydrate in cement paste. Cem Concr Res 30(1):101–116. https://doi.org/10.1016/S0008-8846(99)00209-4
Snoeck D, Velasco LF, Mignon A, Van Vlierberghe S, Dubruel P, Lodewyckx P, De Belie N (2014) The influence of different drying techniques on the water sorption properties of cement-based materials. Cem Concr Res 64:54–62. https://doi.org/10.1016/j.cemconres.2014.06.009
Feldman RF, Sereda PJ (1964) Sorption of water on compacts of bottle-hydrated cement. I. The sorption and length-change isotherms. J Appl Chem 14(2):87–93. https://doi.org/10.1002/jctb.5010140206
Hagymassy J, Odler I, Yudenfreund M, Skalny J, Brunauer S (1972) Pore structure analysis by water vapor adsorption. III. Analysis of hydrated calcium silicates and Portland cements. J Colloid Interference Sci 38(1):20–34. https://doi.org/10.1016/0021-9797(72)90215-9
Odler I, Hagymassy J, Yudenfreund M, Hanna KM, Brunauer S (1972) Pore structure analysis by water vapor adsorption. IV. Analysis of hydrated Portland cement pastes of low porosity. J Colloid Interference Sci 38(1):265–276. https://doi.org/10.1016/0021-9797(72)90242-1
Thommes M, Mitchell S, Perez-Ramırez J (2012) Surface and pore structure assessment of hierarchical MFI zeolites by advanced water and argon sorption studies. J Phys Chem C 116(35):18816–18823. https://doi.org/10.1021/jp3051214
Richardson IG (2008) The calcium silicate hydrates. Cem Concr Res 38(2):137–158. https://doi.org/10.1016/j.cemconres.2007.11.005
Bunkin NF, Kiseleva OA, Lobeyev AV, Movchan TG, Ninham BW, Vinogradova OI (1997) Effect of salts and dissolved gas on optical cavitation near hydrophobic and hydrophilic surfaces. Langmuir 13(11):3024–3028. https://doi.org/10.1021/la960265k
Rasines G, Macías C, Haro M, Jagiello J, Ania CO (2015) Effects of CO2 activation of carbon aerogels leading to ultrahigh micro-meso porosity. Micropor Mesopor Mater 209:18–22. https://doi.org/10.1016/j.micromeso.2015.01.011
Zukai A, Kubů M (2014) High-resolution adsorption analysis of pillared zeolites IPC-3PI and MCM-36. Dalton Trans 27:10558–10565. https://doi.org/10.1039/C4DT00389F
Shimomura M, Yoshida M, Endo A (2017) Influence of free-space calibration using He on the measurement of adsorption isotherms. Adsorption 23(2–3):249–255. https://doi.org/10.1007/s10450-016-9845-2
Horikawa T, Tan SJ, Do DD, Sotowa K, Alcántara-Avila JR, Nicholson D (2017) Temperature dependence of water adsorption on highly graphitized carbon black and highly ordered mesoporous carbon. Carbon 124:271–280. https://doi.org/10.1016/j.carbon.2017.08.067
Horikawa T, Sekida T, Hayashi J, Katoh M, Do DD (2011) A new adsorption/desorption model for water adsorption in porous carbons. Carbon 49(2):416–424. https://doi.org/10.1016/j.carbon.2010.09.038
Yang Q, Sun P, Fumagalli L, Stebunov Y, Haigh S, Zhou Z, Grigorieva I, Wang F, Geim A (2020) Capillary condensation under atomic-scale confinement. Nature 588:250–253. https://doi.org/10.1038/s41586-020-2978-1
Horikawa T, Sakao N, Do DD (2013) Effects of temperature on water adsorption on controlled microporous and mesoporous carbonaceous solids. Carbon 56:183–192. https://doi.org/10.1016/j.carbon.2010.09.038
Bentur A, Milestone NB, Mindess S, Young JF (1979) Creep and drying shrinkage of calcium silicate pastes II. Induced microstructural and chemical changes. Cem Concr Res 8:721–732. https://doi.org/10.1016/0008-8846(78)90081-9
Bentur A, Berger RL, Lawrence FV, Milestone NB, Mindess S, Young JF (1979) Creep and drying shrinkage of calcium silicate pastes III. A hypothesis of irreversible strains. Cem Concr Res 9(1):83–95. https://doi.org/10.1016/0008-8846(79)90098-X
Takahashi K (2015) [Doctoral Dissertation], Effects of mixing and pumping energy on technological and microstructural properties of cement-based mortars. Freiberg, Germany: Technishe Universität Bergakademie Freiberg – Freiberger Forschungshefte A 914
Acknowledgements
We sincerely thank Ms. Mari Kobayashi from Ube Industries for illustrating schematic images of the C-S-H agglomeration units in Fig. 8 and fruitful discussions.
Funding
This research did not receive any specific grant from funding agencies in the public, commercial, or not-for-profit sectors.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of interest
The authors have no conflict of interest directly relevant to the content of this article.
Additional information
Publisher's Note
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Supplementary Information
Below is the link to the electronic supplementary material.
Rights and permissions
About this article
Cite this article
Takahashi, K., Matsui, K., Asamoto, S. et al. Multiscale structural changes and drying shrinkage of Portland cement pastes: effects of a fatty-alcohol-based shrinkage reducing agent. Mater Struct 55, 44 (2022). https://doi.org/10.1617/s11527-022-01889-w
Received:
Accepted:
Published:
DOI: https://doi.org/10.1617/s11527-022-01889-w