Advertisement

Journal of Materials Science

, Volume 53, Issue 8, pp 5958–5972 | Cite as

A comparative study on the pore structure of alkali-activated fly ash evaluated by mercury intrusion porosimetry, N2 adsorption and image analysis

  • Y. Ma
  • G. Wang
  • G. Ye
  • J. Hu
Ceramics

Abstract

In this study, the pore structure of alkali-activated fly ash (AAFA) pastes characterized by different techniques, including mercury intrusion porosimetry (MIP), nitrogen adsorption and image analysis (based on backscattered electron images), was evaluated and compared critically. The degree of reaction of fly ash in AAFA pastes was derived from image analysis. It was found that due to a significant “ink-bottle” effect, the pore diameter of capillary pores derived from MIP was two orders of magnitude smaller than the size determined by image analysis. MIP and nitrogen adsorption results showed different peaks corresponding to the gel pores of AAFA pastes. Based on the experimental results, image analysis is regarded as a reliable technique for the characterization of large pores (> 1 μm) in AAFA pastes. Nitrogen adsorption is more suitable to characterize small pores (< 0.1 μm) in AAFA than MIP, and MIP data should be carefully interpreted, preferably in combination with other characterization techniques.

Notes

Acknowledgements

The authors thank the China Scholarship Council for the financial support to the first author’s study in The Netherlands. We also thank the National High Technology Research and Development Program (“863 Program”, SS2015AA030801), National Natural Science Foundation of China (51402057, 51561135012), Science and Technology Project of Guangdong Province (2016B05051004), Guangzhou Education Bureau Foundation (1201610460), State Key Laboratory of Silicate Materials for Architectures Foundation (SYSJJ2017-05), Pearl River S&T Nova Program of Guangzhou (201506010004) and Australian Research Council Discovery Project (1006016) for funding the project. We would like to thank Professor Klaas van Breugel for his ultimate support and guidance to the project.

References

  1. 1.
    Provis JL, Van Deventer J (2009) Geopolymers: structure, processing, properties and industrial applications. Woodhead Publ. Limited, SawstonCrossRefGoogle Scholar
  2. 2.
    Duxson P, Provis JL, Lukey GC, Van Deventer JSJ (2007) The role of inorganic polymer technology in the development of ‘green concrete’. Cem Concr Res 37:1590–1597CrossRefGoogle Scholar
  3. 3.
    Provis JL, Deventer JSJV (2014) Alkali activated materials. Springer, DordrechtCrossRefGoogle Scholar
  4. 4.
    Romagnoli M (2015) Handbook of alkali-activated cements, mortars and concretesGoogle Scholar
  5. 5.
    Aligizaki KK (2005) Pore structure of cement-based materials: testing, interpretation, and requirements. CRC Press, Boca RatonGoogle Scholar
  6. 6.
    Diamond S (2000) Mercury porosimetry: an inappropriate method for the measurement of pore size distributions in cement-based materials. Cem Concr Res 30:1517–1525CrossRefGoogle Scholar
  7. 7.
    Ma H (2014) Mercury intrusion porosimetry in concrete technology: tips in measurement, pore structure parameter acquisition and application. J Porous Mater 21:207–215CrossRefGoogle Scholar
  8. 8.
    Zeng Q, Li K, Fen-Chong T, Dangla P (2012) Analysis of pore structure, contact angle and pore entrapment of blended cement pastes from mercury porosimetry data. Cem Concr Compos 34:1053–1060CrossRefGoogle Scholar
  9. 9.
    Joyner LG, Barrett EP, Skold R (1951) The determination of pore volume and area distributions in porous substances. II. Comparison between nitrogen isotherm and mercury porosimeter methods. J Am Chem Soc 73:373–380CrossRefGoogle Scholar
  10. 10.
    Gerhardt R (1988) As review of conventional and non-conventional pore characterization techniques. Mrs Online Proceedings Library Archive, 137Google Scholar
  11. 11.
    Aligizaki K (2005) Pore structure of cement-based materials: testing interpretation and requirements. Taylor & Francis, LondonGoogle Scholar
  12. 12.
    Haha MB, Weerdt KD, Lothenbach B (2010) Quantification of the degree of reaction of fly ash. Cem Concr Res 40:1620–1629CrossRefGoogle Scholar
  13. 13.
    Guang YE (2003) Experimental study and numerical simulation of the development of the microstructure and permeability of cementitious materials. J Colloid Interface Sci 262:149–161CrossRefGoogle Scholar
  14. 14.
    Ma Y, Hu J, Ye G (2012) The effect of activating solution on the mechanical strength, reaction rate, mineralogy, and microstructure of alkali-activated fly ash. J Mater Sci 47:4568–4578.  https://doi.org/10.1007/s10853-012-6316-3 CrossRefGoogle Scholar
  15. 15.
    Scrivener K, Snellings R, Lothenbach B (2016) A practical guide to microstructural analysis of cementitious materials. CRC Press, Boca RatonGoogle Scholar
  16. 16.
    Ye G (2003) The microstructure and permeability of cementitious materials. Delft University of Technology, DelftGoogle Scholar
  17. 17.
    Washburn EW (1921) The dynamics of capillary flow. Phys Rev 17:273CrossRefGoogle Scholar
  18. 18.
    Ellison AH, Klemm R, Schwartz AM, Grubb L, Petrash DA (1967) Contact angles of mercury on various surfaces and the effect of temperature. J Chem Eng Data 12:607–609CrossRefGoogle Scholar
  19. 19.
    Gerhardt R (1989) A review of conventional and non-conventional pore characterization techniques. Mater. Res. Soc. Symposium Proceedings, 137, Pore structure and permeability of cementitious materials, Cambridge Univ Press, pp 75–82Google Scholar
  20. 20.
    Barrett EP, Joyner LG, Halenda PP (1951) The determination of pore volume and area distributions in porous substances. I. Computations from nitrogen isotherms. J Am Chem Soc 73:373–380CrossRefGoogle Scholar
  21. 21.
    Scrivener K, Füllmann T, Gallucci E, Walenta G, Bermejo E (2004) Quantitative study of Portland cement hydration by X-ray diffraction/Rietveld analysis and independent methods. Cem Concr Res 34:1541–1547CrossRefGoogle Scholar
  22. 22.
    Diamond S, Leeman ME (1994) Pore size distributions in hardened cement paste by SEM image analysis. Mrs Proceedings, 370Google Scholar
  23. 23.
    Ridler TW, Calvard S (2007) Picture thresholding using an iterative selection method. IEEE Trans Syst Man Cybern 8:630–632Google Scholar
  24. 24.
    Lange DA, Jennings HM, Shah SP (1994) Image analysis techniques for characterization of pore structure of cement-based materials. Cem Concr Res 24:841–853CrossRefGoogle Scholar
  25. 25.
    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. Microporous Mesoporous Mater 126:32–39CrossRefGoogle Scholar
  26. 26.
    Ismail I, Bernal SA, Provis JL, Nicolas RS, Hamdan S, Deventer JSJV (2014) Modification of phase evolution in alkali-activated blast furnace slag by the incorporation of fly ash. Cem Concr Compos 45:125–135CrossRefGoogle Scholar
  27. 27.
    Das S, Yang P, Singh SS, Mertens JCE, Xiao X, Chawla N, Neithalath N (2015) Effective properties of a fly ash geopolymer: synergistic application of X-ray synchrotron tomography, nanoindentation, and homogenization models. Cem Concr Res 78:252–262CrossRefGoogle Scholar
  28. 28.
    Criado M, Fernandez-Jimenez A, de la Torre AG, Aranda MAG, Palomo A (2007) An XRD study of the effect of the SiO2/Na2O ratio on the alkali activation of fly ash. Cem Concr Res 37:671–679CrossRefGoogle Scholar
  29. 29.
    Criado M, Fernandez-Jimenez A, Palomo A, Sobrados I, Sanz J (2008) Effect of the Sio(2)/Na2O ratio on the alkali activation of fly ash. Part II: Si-29 MAS-NMR Survey. Microporous Mesoporous Mater 109:525–534CrossRefGoogle Scholar
  30. 30.
    Rees CA, Provis JL, Lukey GC, van Deventer JSJ (2007) In situ ATR-FTIR study of the early stages of fly ash geopolymer gel formation. Langmuir 23:9076–9082CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC, part of Springer Nature 2018

Authors and Affiliations

  1. 1.Guangzhou University - Tamkang University Joint Research, Center for Engineering Structure Disaster Prevention and ControlGuangzhou UniversityGuangzhouPeople’s Republic of China
  2. 2.Centre for Future Materials, Faculty of Health, Engineering and SciencesUniversity of Southern QueenslandToowoombaAustralia
  3. 3.Department Materials and Environment, Faculty of Civil Engineering and GeosciencesDelft University of TechnologyDelftThe Netherlands
  4. 4.Department of Structural EngineeringGhent UniversityGhentBelgium
  5. 5.School of Materials Science and EngineeringSouth China University of TechnologyGuangzhouPeople’s Republic of China

Personalised recommendations