Technical Papers
Mar 31, 2023

Influence of Process Variables on Shrinkage in Low-Calcium Fly-Ash Geopolymers

Publication: Journal of Materials in Civil Engineering
Volume 35, Issue 6

Abstract

The influence of process variables such as curing temperature and relative humidity (RH) on the shrinkage of alkali-activated fly ash (AAF) is examined in this work. The ambient conditions are varied after an initial accelerated moist curing at high-temperature. An analysis interlinking the effects of curing on AAF strength, shrinkage, reaction product content, and porosity is performed. Strength achieved and the pore structure formed for the different curing conditions depend upon the sodium alumino-silicate (N-A-S-H) gel content formed in the AAF. While water is not directly combined in the formation of N-A-S-H gel, its content is sensitive to the availability of moisture. The moisture loss due to drying during the geopolymerization reduces the N-A-S-H content formed in the AAF. Compared to the continuous moist curing at elevated temperature, there is a decrease in the N-A-S-H content on lowering the temperature or drying produced by the decrease in RH. Reducing temperature and RH following initial accelerated curing has the beneficial effect of reducing the shrinkage compared to drying at a higher temperature. Reduction in the N-A-S-H content due to decrease in temperature after the accelerated curing is more significant than the drying on lowering the RH to 50%. The autogenous shrinkage measured under sealed conditions contributes significantly to the total shrinkage in AAF. The shrinkage in the AAF is significantly lower than a comparable cement paste. While shrinkage is produced by drying, the moisture loss and shrinkage relationship is not unique. The shrinkage produced by moisture loss due to drying is primarily influenced by the pore structure formed in the AAF, which also depends on the N-A-S-H content. The influences of temperature and humidity on the strength, pore structure and shrinkage are determined by the N-A-S-H formed in the AAF.

Get full access to this article

View all available purchase options and get full access to this article.

Data Availability Statement

Some or all data, models, or codes that support the findings of this study are available from the corresponding author upon reasonable request.

Acknowledgments

The lead author would like to acknowledge support from the Ministry of tribal affairs, India, under the scheme “National Fellowship and Scholarship for Higher Education of ST students.”

References

Assi, L., S. A. Ghahari, E. E. Deaver, D. Leaphart, and P. Ziehl. 2016. “Improvement of the early and final compressive strength of fly ash-based geopolymer concrete at ambient conditions.” Constr. Build. Mater. 123 (Oct): 806–813. https://doi.org/10.1016/j.conbuildmat.2016.07.069.
ASTM. 2007. Standard test method for drying shrinkage of mortar containing hydraulic cement. ASTM C596-18. West Conshohocken, PA: ASTM.
ASTM. 2010. Standard specification for coal fly ash and raw or calcined natural pozzolan for use. ASTM C618-19. West Conshohocken, PA: ASTM.
Aughenbaugh, K. L., T. Williamson, and M. C. G. Juenger. 2014. “Critical evaluation of strength prediction methods for alkali-activated fly ash.” Mater. Struct./Materiaux et Constr. 48 (3): 607–620.
Baroghel-Bouny, V., P. Mounanga, A. Khelidj, A. Loukili, and N. Rafaï. 2006. “Autogenous deformations of cement pastes: Part II. W/C effects, micro-macro correlations, and threshold values.” Cem. Concr. Res. 36 (1): 123–136. https://doi.org/10.1016/j.cemconres.2004.10.020.
Beltzung, F., and F. H. Wittmann. 2005. “Role of disjoining pressure in cement-based materials.” Cem. Concr. Res. 35 (12): 2364–2370. https://doi.org/10.1016/j.cemconres.2005.04.004.
Bernardo, G., A. Telesca, and G. L. Valenti. 2006. “A porosimetric study of calcium sulfoaluminate cement pastes cured at early ages.” Cem. Concr. Res. 36 (6): 1042–1047. https://doi.org/10.1016/j.cemconres.2006.02.014.
Bhagath Singh, G. V. P., and K. V. L. Subramaniam. 2016a. “Direct decomposition X-ray diffraction method for amorphous phase quantification and glassy phase determination in binary blends of siliceous fly ash and hydrated cement.” J. Sustainable Cem.-Based Mater. 6 (2): 111–125. https://doi.org/10.1080/21650373.2016.1177478.
Bhagath Singh, G. V. P., and K. V. L. Subramaniam. 2016b. “Method for direct determination of glassy phase dissolution in hydrating fly ash-cement system using x-ray diffraction.” J. Am. Ceram. Soc. 100 (1): 403–412. https://doi.org/10.1111/jace.14486.
Bhagath Singh, G. V. P., and K. V. L. Subramaniam. 2016c. “Quantitative XRD study of amorphous phase in alkali activated low calcium siliceous fly ash.” Constr. Build. Mater. 124 (Oct): 139–147. https://doi.org/10.1016/j.conbuildmat.2016.07.081.
Bhagath Singh, G. V. P., and K. V. L. Subramaniam. 2017a. “Evaluation of sodium content and sodium hydroxide molarity on compressive strength of alkali activated low-calcium fly ash.” Cem. Concr. Compos. 81 (Aug): 122–132. https://doi.org/10.1016/j.cemconcomp.2017.05.001.
Bhagath Singh, G. V. P., and K. V. L. Subramaniam. 2017b. “Role of reactive alumina and reactive oxide ratios on strength development in alkaline activation of low-calcium fly ash.” In Vol. 2 of Proc., Int. Conf. on Advances in Construction Materials and Systems, 243–250. Paris: RILEM Publications SARL.
Bhagath Singh, G. V. P., and K. V. L. Subramaniam. 2017c. “Role of total reactive oxide ratios on strength development in activated fly ash.” In Proc., Int. Conf. on Advances in Sustainable Construction Materials & Civil Engineering Systems (ASCMCES-17). Les Ulis, France: EDP Sciences. https://doi.org/10.1051/matecconf/201712002014.
Bhagath Singh, G. V. P., and K. V. L. Subramaniam. 2018. “Characterization of Indian fly ashes using different experimental techniques.” Indian Concr. J. 92 (3): 10–23.
Bhagath Singh, G. V. P., and K. V. L. Subramaniam. 2019a. “Effect of active components on strength development in alkali-activated low calcium fly ash cements.” J. Sustainable Cem.-Based Mater. 8 (1): 1–19. https://doi.org/10.1080/21650373.2018.1520657.
Bhagath Singh, G. V. P., and K. V. L. Subramaniam. 2019b. “Influence of processing temperature on the reaction product and strength gain in alkali-activated fly ash.” Cem. Concr. Compos. 95 (Oct): 10–18. https://doi.org/10.1016/j.cemconcomp.2018.10.010.
Bhagath Singh, G. V. P., and K. V. L. Subramaniam. 2020. “Evaluation of total reactive oxide ratios and working solution ratios on strength development in fly ash–based geopolymers.” J. Mater. Civ. Eng. 32 (4): 04020051. https://doi.org/10.1061/(ASCE)MT.1943-5533.0003109.
BIS (Bureau of Indian Standards). 2005. Methods of physical tests for hydraulic cement Part 6: Determination of compressive strength of hydraulic cement other than masonry cement (first revision). IS: 4031. New Delhi, India: BIS.
BIS (Bureau of Indian Standards). 2013. Specification for Pulverized fuel ash, Part-1: For use as Pozzolana in cement, cement mortar and concrete. IS:3812. New Delhi, India: BIS.
Chindaprasirt, P., U. Rattanasak, P. Vongvoradit, and S. Jenjirapanya. 2012. “Thermal treatment and utilization of Al-rich waste in high calcium fly ash geopolymeric materials.” Int. J. Miner. Metall. Mater. 19 (9): 872–878. https://doi.org/10.1007/s12613-012-0641-z.
Cong, X., and R. J. Kirkpatrick. 1995. “Effects of the temperature and relative humidity on the structure of CSH gel.” Cem. Concr. Res. 25 (6): 1237–1245. https://doi.org/10.1016/0008-8846(95)00116-T.
Cook, R. A., and K. C. Hover. 1999. “Mercury porosimetry of hardened cement pastes.” Cem. Concr. Res. 29 (6): 933–943. https://doi.org/10.1016/S0008-8846(99)00083-6.
Corp, M. I. 2001. “An introduction to the physical characterization of materials by mercury intrusion porosimetry with emphasis on reduction and presentation of experimental data Paul A. Webb Norcross, Georgia.” Mercury 22 (Jan): 1–23.
Davidovits, J. 2020. Geopolymer chemistry and applications. 5th ed. Saint-Quentin, France: Institut Géopolymère.
Dong, H., P. Gao, and G. Ye. 2017. “Characterization and comparison of capillary pore structures of digital cement pastes.” Mater. Struct./Mater. Constr. 50 (2): 1–12. https://doi.org/10.1617/s11527-017-1023-9.
Duxson, P., A. Fernández-Jiménez, J. L. Provis, G. C. Lukey, A. Palomo, and J. S. J. Van Deventer. 2007. “Geopolymer technology: The current state of the art.” J. Mater. Sci. 42 (9): 2917–2933. https://doi.org/10.1007/s10853-006-0637-z.
Gunasekera, C., S. Setunge, and D. W. Law. 2019. “Creep and drying shrinkage of different fly-ash-based geopolymers.” ACI Mater. J. 116 (1): 39–49. https://doi.org/10.14359/51706941.
Habert, G., J. B. D’Espinose De Lacaillerie, and N. Roussel. 2011. “An environmental evaluation of geopolymer based concrete production: Reviewing current research trends.” J. Cleaner Prod. 19 (11): 1229–1238. https://doi.org/10.1016/j.jclepro.2011.03.012.
Hajimohammadi, A., and J. S. J. van Deventer. 2017. “Characterisation of one-part geopolymer binders made from fly ash.” Waste Biomass Valorization 8 (1): 225–233. https://doi.org/10.1007/s12649-016-9582-5.
Hanumananaik, M., M. S. K. Reddy, and K. V. L. Subramaniam. 2022. “High-temperature performance of low-calcium fly ash–based geopolymers.” J. Mater. Civ. Eng. 34 (5): 04022040. https://doi.org/10.1061/(ASCE)MT.1943-5533.0004181.
Hill, R. J., and C. J. Howard. 1987. “Quantitative phase analysis from neutron powder diffraction data using the Rietveld method.” J. Appl. Crystallogr. 20 (6): 467–474. https://doi.org/10.1107/S0021889887086199.
Hojati, M., F. Rajabipour, and A. Radlińska. 2019. “Effect of activator, curing and humidity on drying shrinkage of alkali-activated fly ash.” Green Mater. 7 (2): 71–83. https://doi.org/10.1680/jgrma.18.00069.
Komljenović, M. 2015. “Mechanical strength and Young’s modulus of alkali-activated cement-based binders.” In Handbook of alkali-activated cements, mortars and concretes, 171–215. Cambridge, MA: Woodhead Publishing.
Leong, H. Y, D. E. L. Ong, J. G. Sanjayan, and A. Nazari. 2016. “The effect of different Na2O and K2O ratios of alkali activator on compressive strength of fly ash based-geopolymer.” Constr. Build. Mater. 106 (Mar): 500–511. https://doi.org/10.1016/j.conbuildmat.2015.12.141.
Ling, Y., K. Wang, and C. Fu. 2019. “Shrinkage behavior of fly ash based geopolymer pastes with and without shrinkage reducing admixture.” Cem. Concr. Compos. 98 (Feb): 74–82. https://doi.org/10.1016/j.cemconcomp.2019.02.007.
Lloyd, R. R., J. L. Provis, K. J. Smeaton, and J. S. J. van Deventer. 2009. “Spatial distribution of pores in fly ash-based inorganic polymer gels visualised by Wood’s metal intrusion.” Microporous Mesoporous Mater. 126 (1–2): 32–39. https://doi.org/10.1016/j.micromeso.2009.05.016.
Ma, Y., and G. Ye. 2015. “The shrinkage of alkali activated fly ash.” Cem. Concr. Res. 68 (Feb): 75–82. https://doi.org/10.1016/j.cemconres.2014.10.024.
Madsen, I. C., N. V. Y. Scarlett, and A. Kern. 2011. “Description and survey of methodologies for the determination of amorphous content via X-ray powder diffraction.” Z. Kristallogr. 226 (12): 944–955. https://doi.org/10.1524/zkri.2011.1437.
Mclellan, B. C., R. P. Williams, J. Lay, A. Van Riessen, and G. D. Corder. 2011. “Costs and carbon emissions for geopolymer pastes in comparison to ordinary portland cement.” J. Cleaner Prod. 19 (9–10): 1080–1090. https://doi.org/10.1016/j.jclepro.2011.02.010.
Pacheco-Torgal, F., Z. Abdollahnejad, A. F. Camões, M. Jamshidi, and Y. Ding. 2012. “Durability of alkali-activated binders: A clear advantage over portland cement or an unproven issue?” Constr. Build. Mater. 30 (May): 400–405. https://doi.org/10.1016/j.conbuildmat.2011.12.017.
Pawley, G. S. 1981. “Unit-cell refinement from powder diffraction scans.” J. Appl. Crystallogr. 14 (6): 357–361. https://doi.org/10.1107/S0021889881009618.
Provis, J. L., and J. S. J. Van Deventer. 2009. Geopolymers Structure, processing, properties and industrial applications. Oxford, UK: Woodhead Publishing Limited.
Reddy, K. C., and K. V. L. Subramaniam. 2020. “Quantitative phase analysis of slag hydrating in an alkaline environment.” J. Appl. Crystallogr. 53 (2): 424–434. https://doi.org/10.1107/S1600576720001399.
Reddy, K. C., and K. V. L. Subramaniam. 2021. “Investigation on the roles of solution-based alkali and silica in activated low-calcium fly ash and slag blends.” Cem. Concr. Compos. 123 (Jul): 104175. https://doi.org/10.1016/j.cemconcomp.2021.104175.
Riello, P. 2004. “Quantitative analysis of amorphous fraction in the study of the microstructure of semi-crystalline materials.” In Vol. 68 of Diffraction analysis of the microstructure of materials, edited by E. J. Mittemeijer and P. Scardi. Berlin: Springer.
Rietveld, H. M. 1969. “A profile refinement method for nuclear and magnetic structures.” J. Appl. Crystallogr. 2 (2): 65–71. https://doi.org/10.1107/S0021889869006558.
Ryu, G. S., Y. B. Lee, K. T. Koh, and Y. S. Chung. 2013. “The mechanical properties of fly ash-based geopolymer concrete with alkaline activators.” Constr. Build. Mater. 47 (Oct): 409–418. https://doi.org/10.1016/j.conbuildmat.2013.05.069.
Sagoe-Crentsil, K., T. Brown, and A. Taylor. 2013. “Drying shrinkage and creep performance of geopolymer concrete.” J. Sustainable Cem.-Based Mater. 2 (1): 35–42. https://doi.org/10.1080/21650373.2013.764963.
Šmilauer, V., P. Hlaváček, F. Škvára, R. Šulc, L. Kopecký, and J. Němeček. 2011. “Micromechanical multiscale model for alkali activation of fly ash and metakaolin.” J. Mater. Sci. 46 (20): 6545–6555. https://doi.org/10.1007/s10853-011-5601-x.
Snellings, R., A. Salze, and K. L. Scrivener. 2014. “Use of X-ray diffraction to quantify amorphous supplementary cementitious materials in anhydrous and hydrated blended cements.” Cem. Concr. Res. 64 (Oct): 89–98. https://doi.org/10.1016/j.cemconres.2014.06.011.
Songpiriyakij, S., T. Kubprasit, C. Jaturapitakkul, and P. Chindaprasirt. 2010. “Compressive strength and degree of reaction of biomass- and fly ash-based geopolymer.” Constr. Build. Mater. 24 (3): 236–240. https://doi.org/10.1016/j.conbuildmat.2009.09.002.
Stetsko, Y. P., N. Shanahan, H. Deford, and A. Zayed. 2017. “Quantification of supplementary cementitious content in blended Portland cement using an iterative Rietveld-PONKCS technique.” J. Appl. Crystallogr. 50 (2): 498–507. https://doi.org/10.1107/S1600576717002965.
Thomas, R. J., D. Lezama, and S. Peethamparan. 2017. “On drying shrinkage in alkali-activated concrete: Improving dimensional stability by aging or heat-curing.” Cem. Concr. Res. 91 (Jan): 13–23. https://doi.org/10.1016/j.cemconres.2016.10.003.
Wallah, S. E., and B. V. Rangan. 2006. “Low calcium fly ash-based geopolymer concrete: Long-term properties.” In Research report GC 2 faculty of engineering. Perth, WA, Australia: Curtin Univ. of Technology Perth.
Warangkana, S., T. Nawa, and P. Termkhajornkit. 2008. “Influence of relative humidity on compressive strength of fly ash cement paste.” J. Struct. Constr. Eng. 73 (631): 1433–1441. https://doi.org/10.3130/aijs.73.1433.
Wongpa, J., K. Kiattikomol, C. Jaturapitakkul, and P. Chindaprasirt. 2010. “Compressive strength, modulus of elasticity, and water permeability of inorganic polymer concrete.” Mater. Des. 31 (10): 4748–4754. https://doi.org/10.1016/j.matdes.2010.05.012.
Zhang, Q., Z. Kang, Y. Ling, H. Chen, and K. Li. 2021. “Influence of temperature on the moisture transport in concrete.” Crystals 11 (1): 69. https://doi.org/10.3390/cryst11010069.

Information & Authors

Information

Published In

Go to Journal of Materials in Civil Engineering
Journal of Materials in Civil Engineering
Volume 35Issue 6June 2023

History

Received: Apr 21, 2022
Accepted: Oct 14, 2022
Published online: Mar 31, 2023
Published in print: Jun 1, 2023
Discussion open until: Aug 31, 2023

Permissions

Request permissions for this article.

Authors

Affiliations

Research Scholar, Dept. of Civil Engineering, Indian Institute of Technology Hyderabad, Hyderabad, Telangana 502285, India. ORCID: https://orcid.org/0000-0002-0970-371X. Email: [email protected]
Professor, Dept. of Civil Engineering, Indian Institute of Technology Hyderabad, Hyderabad, Telangana 502285, India (corresponding author). ORCID: https://orcid.org/0000-0002-5995-0911. Email: [email protected]

Metrics & Citations

Metrics

Citations

Download citation

If you have the appropriate software installed, you can download article citation data to the citation manager of your choice. Simply select your manager software from the list below and click Download.

View Options

Get Access

Access content

Please select your options to get access

Log in/Register Log in via your institution (Shibboleth)
ASCE Members: Please log in to see member pricing

Purchase

Save for later Information on ASCE Library Cards
ASCE Library Cards let you download journal articles, proceedings papers, and available book chapters across the entire ASCE Library platform. ASCE Library Cards remain active for 24 months or until all downloads are used. Note: This content will be debited as one download at time of checkout.

Terms of Use: ASCE Library Cards are for individual, personal use only. Reselling, republishing, or forwarding the materials to libraries or reading rooms is prohibited.
ASCE Library Card (5 downloads)
$105.00
Add to cart
ASCE Library Card (20 downloads)
$280.00
Add to cart
Buy Single Article
$35.00
Add to cart

Get Access

Access content

Please select your options to get access

Log in/Register Log in via your institution (Shibboleth)
ASCE Members: Please log in to see member pricing

Purchase

Save for later Information on ASCE Library Cards
ASCE Library Cards let you download journal articles, proceedings papers, and available book chapters across the entire ASCE Library platform. ASCE Library Cards remain active for 24 months or until all downloads are used. Note: This content will be debited as one download at time of checkout.

Terms of Use: ASCE Library Cards are for individual, personal use only. Reselling, republishing, or forwarding the materials to libraries or reading rooms is prohibited.
ASCE Library Card (5 downloads)
$105.00
Add to cart
ASCE Library Card (20 downloads)
$280.00
Add to cart
Buy Single Article
$35.00
Add to cart

Media

Figures

Other

Tables

Share

Share

Copy the content Link

Share with email

Email a colleague

Share