Skip to main content
SpringerLink
Log in

Does synthesized C-S-H seed promote nucleation in alkali activated fly ash-slag geopolymer binder?

  • Original Article
  • Published:
Materials and Structures Aims and scope Submit manuscript

Abstract

Understanding the effects of nucleation seeds on reaction kinetics and microstructures of alkali activated binders (AABs) is important since it will help us control both early-age and long-term properties. For example, in the calcium-containing AABs, calcium silicate hydrate/calcium aluminosilicate hydrate (C-S-H/C-A-S-H) seeds have been proposed by others to act as nucleation sites to promote formation of geopolymer gel. In this study, we examined the nucleation effects by adding synthesized C-S-H and C-A-S-H seeds into class F fly ash-slag mixes activated both by potassium hydroxide and by potassium silicate solutions. From both calorimetry and ultrasonic wave reflection tests, we found seeding to accelerate reaction of the hydroxide activated binder but decelerate that of the silicate activated binder. Based on further chemical treatments and Fourier-transform infrared spectroscopic characterization, we found the acceleration in the hydroxide binder was due to enhanced formation of C-S-H/C-A-S-H, while the deceleration in the silicate binder was due to decreased formation of K-A-S-H gel despite the enhanced formation of C-S-H/C-A-S-H. Additionally, in both types of binders, we found dissolution of fly ash precursor was enhanced. Evidence in this study suggests that C-S-H seeds act as nucleation sites for further precipitation of C-S-H/C-A-S-H but not for formation of geopolymer gel.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9
Fig. 10

Similar content being viewed by others

References

  1. Hubler MH, Thomas JJ, Jennings HM (2011) Influence of nucleation seeding on the hydration kinetics and compressive strength of alkali activated slag paste. Cem Concr Res 41(8):842–846. https://doi.org/10.1016/j.cemconres.2011.04.002

    Article  Google Scholar 

  2. Thomas JJ, Jennings HM, Chen JJ (2009) Influence of nucleation seeding on the hydration mechanisms of tricalcium silicate and cement. J Phys Chem C 113(11):4327–4334. https://doi.org/10.1021/jp809811w

    Article  Google Scholar 

  3. Provis JL, Bernal SA (2014) Geopolymers and related alkali-activated materials. Annu Rev Mater Res 44(1):299–327. https://doi.org/10.1146/annurev-matsci-070813-113515

    Article  Google Scholar 

  4. Rees CA, Provis JL, Lukey GC, van Deventer JSJ (2008) The mechanism of geopolymer gel formation investigated through seeded nucleation. Colloid Surf A 318(1–3):97–105. https://doi.org/10.1016/j.colsurfa.2007.12.019

    Article  Google Scholar 

  5. Hajimohammadi A, Provis JL, van Deventer JSJ (2011) Time-resolved and spatially-resolved infrared spectroscopic observation of seeded nucleation controlling geopolymer gel formation. J Colloid Interf Sci 357(2):384–392. https://doi.org/10.1016/j.jcis.2011.02.045

    Article  Google Scholar 

  6. Lloyd RR, Provis JL, van Deventer JSJ (2009) Microscopy and microanalysis of inorganic polymer cements. 2: The gel binder. J Mater Sci 44(2):620–631. https://doi.org/10.1007/s10853-008-3078-z

    Article  Google Scholar 

  7. Puligilla S, Chen X, Mondal P (2018) Understanding the role of silicate concentration on the early-age reaction kinetics of a calcium containing geopolymeric binder. Constr Build Mater 191:206–215

    Article  Google Scholar 

  8. Chen X, Sutrisno A, Zhu L, Struble LJ (2017) Setting and nanostructural evolution of metakaolin geopolymer. J Am Ceram Soc 100(5):2285–2295. https://doi.org/10.1111/jace.14641

    Article  Google Scholar 

  9. White CE, Provis JL, Llobet A, Proffen T, van Deventer JSJ (2011) Evolution of local structure in geopolymer gels: an in situ neutron pair distribution function analysis. J Am Ceram Soc 94(10):3532–3539. https://doi.org/10.1111/j.1551-2916.2011.04515.x

    Article  Google Scholar 

  10. Lloyd RR, Provis JL, Smeaton KJ, van Deventer JSJ (2009) Spatial distribution of pores in fly ash-based inorganic polymer gels visualised by Wood’s metal intrusion. Micropor Mesopor Mater 126(1–2):32–39. https://doi.org/10.1016/j.micromeso.2009.05.016

    Article  Google Scholar 

  11. van Jaarsveld JGS, van Deventer JSJ (1999) Effect of the alkali metal activator on the properties of fly ash-based geopolymers. Ind Eng Chem Res 38(10):3932–3941. https://doi.org/10.1021/ie980804b

    Article  Google Scholar 

  12. Bernal SA, Provis JL, Rose V, Mejía de Gutierrez R (2011) Evolution of binder structure in sodium silicate-activated slag-metakaolin blends. Cem Concr Compos 33(1):46–54. https://doi.org/10.1016/j.cemconcomp.2010.09.004

    Article  Google Scholar 

  13. Fernández-Jimenez A, de la Torre AG, Palomo A, López-Olmo G, Alonso MM, Aranda MAG (2006) Quantitative determination of phases in the alkali activation of fly ash. Part I. Potential ash reactivity. Fuel 85(5–6):625–634

    Article  Google Scholar 

  14. Yip CK, Lukey GC, Provis JL, van Deventer JSJ (2008) Effect of calcium silicate sources on geopolymerisation. Cem Concr Res 38(4):554–564. https://doi.org/10.1016/j.cemconres.2007.11.001

    Article  Google Scholar 

  15. Kumar S, Kumar R, Mehrotra SP (2010) Influence of granulated blast furnace slag on the reaction, structure and properties of fly ash based geopolymer. J Mater Sci 45(3):607–615. https://doi.org/10.1007/s10853-009-3934-5

    Article  Google Scholar 

  16. Yip CK, van Deventer JSJ (2003) Microanalysis of calcium silicate hydrate gel formed within a geopolymeric binder. J Mater Sci 38(18):3851–3860. https://doi.org/10.1023/A:1025904905176

    Article  Google Scholar 

  17. Temuujin J, van Riessen A, Williams R (2009) Influence of calcium compounds on the mechanical properties of fly ash geopolymer pastes. J Hazard Mater 167(1–3):82–88. https://doi.org/10.1016/j.jhazmat.2008.12.121

    Article  Google Scholar 

  18. Puligilla S, Mondal P (2013) Role of slag in microstructural development and hardening of fly ash-slag geopolymer. Cem Concr Res 43:70–80. https://doi.org/10.1016/j.cemconres.2012.10.004

    Article  Google Scholar 

  19. Chen X, Sutrisno A, Struble LJ (2018) Effects of calcium on setting mechanism of metakaolin-based geopolymer. J Am Ceram Soc 101(2):957–968. https://doi.org/10.1111/jace.15249

    Article  Google Scholar 

  20. Puligilla S, Mondal P (2015) Co-existence of aluminosilicate and calcium silicate gel characterized through selective dissolution and FTIR spectral subtraction. Cem Concr Res 70:39–49. https://doi.org/10.1016/j.cemconres.2015.01.006

    Article  Google Scholar 

  21. Lee W, Van Deventer J (2002) The effect of ionic contaminants on the early-age properties of alkali-activated fly ash-based cements. Cem Concr Res 32(4):577–584

    Article  Google Scholar 

  22. Puligilla S (2017) Understanding the role of calcium on the reaction mechanism of geopolymer cements through addition of nucleation seeds. University of Illinois at Urbana-Champaign, Champaign

    Google Scholar 

  23. Begarin F, Garrault S, Nonat A, Nicoleau L (2011) Hydration of alite containing aluminium. Adv Appl Ceram 110(3):127–130. https://doi.org/10.1179/1743676110Y.0000000007

    Article  Google Scholar 

  24. Hunnicutt W, Struble L, Mondal P (2017) Effect of synthesis procedure on carbonation of calcium-silicate-hydrate. J Am Ceram Soc 100(8):3736–3745. https://doi.org/10.1111/jace.14899

    Article  Google Scholar 

  25. Suraneni P, Puligilla S, Kim E, Chen X, Struble L, Mondal P, Kim EH, Struble LJ (2014) Monitoring setting of geopolymers. Adv Civ Eng Mater 3:177–192

    Google Scholar 

  26. Chen X, Meawad A, Struble LJ (2014) Method to stop geopolymer reaction. J Am Ceram Soc 97(10):3270–3275

    Article  Google Scholar 

  27. Yu P, Kirkpatrick RJ, Poe B, McMillan PF, Cong X (1999) Structure of calcium silicate hydrate (C-S-H): near-, mid-, and far-infrared spectroscopy. J Am Ceram Soc 82(3):742–748. https://doi.org/10.1111/j.1151-2916.1999.tb01826.x

    Article  Google Scholar 

  28. Zhu W, Chen X, Struble LJ, Yang E-H (2018) Characterization of calcium-containing phases in alkali-activated municipal solid waste incineration bottom ash binder through chemical extraction and deconvoluted Fourier transform infrared spectra. J Clean Prod 192:782–789. https://doi.org/10.1016/j.jclepro.2018.05.049

    Article  Google Scholar 

  29. Fernández-Jiménez A, Palomo A (2005) Mid-infrared spectroscopic studies of alkali-activated fly ash structure. Micropor Mesopor Mater 86(1):207–214

    Article  Google Scholar 

  30. García-Lodeiro I, Fernández-Jiménez A, Blanco MT, Palomo A (2008) FTIR study of the sol–gel synthesis of cementitious gels: C-S-H and N-A-S-H. J Sol-Gel Sci Technol 45(1):63–72. https://doi.org/10.1007/s10971-007-1643-6

    Article  Google Scholar 

  31. Garcia-Lodeiro I, Palomo A, Fernández-Jiménez A, Macphee DE (2011) Compatibility studies between N-A-S-H and C-A-S-H gels Study in the ternary diagram Na2O–CaO–Al2O3–SiO2–H2O. Cem Concr Res 41(9):923–931

    Article  Google Scholar 

  32. Oh JE, Moon J, Oh S-G, Clark SM, Monteiro PJM (2012) Microstructural and compositional change of NaOH-activated high calcium fly ash by incorporating Na-aluminate and co-existence of geopolymeric gel and C-S-H(I). Cem Concr Res 42(5):673–685

    Article  Google Scholar 

Download references

Acknowledgements

The authors would like to thank Dipobrato Sarbapalli and Professor Leslie J. Struble at University of Illinois for their invaluable comments and thank Professor John S. Popovis at University of Illinois for his substantial help with UWR measurements. The SEM analysis was carried out in the Frederick Seitz Materials Research Laboratory Central Facilities at University of Illinois. This study was funded through an NSF Grant (No. #1538432).

Author information

Authors and Affiliations

  1. SpaceX, 1 Rocket Road, Hawthorne, CA, 90250, USA

    Sravanthi Puligilla

  2. Department of Civil and Environmental Engineering, University of Delaware, Newark, DE, 19716, USA

    Xu Chen & Paramita Mondal

Authors
  1. Sravanthi Puligilla
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Xu Chen
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Paramita Mondal
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Xu Chen.

Ethics declarations

Conflict of interest

The authors declare that they have no conflict of interest.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Appendix

Appendix

See Figs. 9 and 10.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Puligilla, S., Chen, X. & Mondal, P. Does synthesized C-S-H seed promote nucleation in alkali activated fly ash-slag geopolymer binder?. Mater Struct 52, 65 (2019). https://doi.org/10.1617/s11527-019-1368-3

Download citation

  • Received:

  • Accepted:

  • Published:

  • DOI: https://doi.org/10.1617/s11527-019-1368-3

Keywords

Search

Navigation