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Performance of Low-Grade Calcined Clays as Supplementary Cementitious Material in Relation to their Geological Characteristics

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Clays and Clay Minerals

Abstract

Calcined clays are used as a supplementary cementitious material (SCM) because, as hydrated aluminosilicates of the phyllosilicate group, they can be activated thermally, promoting dehydroxylation and structural disorder, i.e. making them reactive. The main effect of using calcined clay as an SCM is that CO2 emissions into the atmosphere are reduced by the reduction in the clinker/cement factor due to substitution of a proportion of clinker by calcined clay. Clays rich in kaolinite (1:1) group minerals offer most promise in terms of thermal activation. However, increased costs caused by demand for kaolinite from other industries means that type 2:1 calcined clays and mixtures of them have begun to be investigated as possible pozzolanic materials. The physical, chemical, and mineralogical characteristics that control the performance of these calcined clays as SCMs are still under discussion. Few in-depth studies of the behavior of these characteristics have been reported. The origin and geological history of raw materials, as well as their impact on the thermal activation and performance as SCM, are not well understood or, in some cases, have not been considered. The objective of the current work, therefore, was to study multicomponent clays from metamorphic rocks with low-grade kaolinite (<50%) from a tropical region of Colombia for possible use as SCMs. The clay deposit was identified by geological exploration techniques and classified in depth according to horizons of the weathering profile. The samples were extracted from the first 50 m of the deposit and characterized physically, chemically, and mineralogically; they were calcined at 650, 750, and 850°C; their degree of alteration was estimated by the Chemical Index of Alteration (CIA); and their performance as an SCM was evaluated by the Strength Activity Index (SAI) and Frattini test. As a main result, a relationship was found between the weathering profile of the deposit and the CIA of raw clays, which confirmed the high weathering and degree of alteration of the parent rock in the deposit (weathered rock and residual soil with a CIA > 80%). Furthermore, pozzolanic (physical and chemical) tests demonstrated the potential use of calcined clays from this deposit as SCMs, as well as their thermal activation at low temperature (≤750°C). In addition, the pozzolanic activity increased with the kaolinite/(muscovite+illite+vermiculite) ratio mainly, and, in turn, the thermal activation temperature increased with the mica and type 2:1 clay content.

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All data generated or analysed during this study are included in the supplementary information files. Data of Figures are presented in the attached supplementary material in PDF format named “Supplemental Material 1” and spreadsheets named " Supplemental Material 2".

References

  • AENOR (2011). UNE-EN 196-5 Cement test methods Part 5: Pozzolanicity test for pozzolanic cements. Spanish Association of Standardization and Certification (AENOR), Madrid.

    Google Scholar 

  • Alujas, A., Fernández, R., Quintana, R., Scrivener, K. L., & Martirena, F. (2015). Pozzolanic reactivity of low grade kaolinitic clays: Influence of calcination temperature and impact of calcination products on OPC hydration. Applied Clay Science, 108, 94–101. https://doi.org/10.1016/j.clay.2015.01.028

    Article  Google Scholar 

  • Alvarado, A., Mata, R., & Chinchilla, M. (2014). Clays identified in soils of Costa Rica at a generalized level during the period 1931–2014: I. History, methodology of analysis, and mineralogy of clays in soils derived from volcanic ash. Agronomía Costarricense, 38(1), 75–106 (in Spanish). https://doi.org/10.15517/rac.v38i1.15160

  • Antoni, M. (2013). Investigation of cement substitution by combined addition of calcined clays and limestone. PhD thesis, Lausanne Federal Polytechnic School, Lausanne, Switzerland, vol 6001.

  • Aristizábal, E., Roser, B., & Yokota, S. (2005). Tropical chemical weathering of hillslope deposits and bedrock source in the Aburrá Valley, northern Colombian Andes. Engineering Geology, 81, 389–406. https://doi.org/10.1016/j.enggeo.2005.08.001

    Article  Google Scholar 

  • ASTM Committee (2002). ASTM C109/C109M-02 Standard test method for compressive strength of hydraulic cement mortars. ASTM International. https://doi.org/10.1520/C0109_C0109M-21

    Book  Google Scholar 

  • ASTM Committee (2018a). ASTM C1709-18 Standard Guide for Evaluation of Alternative Supplementary Cementitious Materials (ASCM) for Use in Concrete. ASTM International. https://doi.org/10.1520/C1709-18

  • ASTM Committee. (2018b). ASTM C311-18 Standard test methods for sampling and testing fly ash or natural pozzolans for use in Portland cement concrete. ASTM International. https://doi.org/10.1520/C0311_C0311M-18

    Book  Google Scholar 

  • ASTM Committee. (2019). ASTM C618-19 Standard specification for coal fly ash and raw or calcined natural pozzolan for use in concrete. ASTM International. https://doi.org/10.1520/C0618

    Book  Google Scholar 

  • Besoain, E. (1985). Mineralogy of soil clays. Inter-American Center of Agricultural Documentation and Information CIDIA, Inter-American Institute of Cooperation for Agriculture IICA (Eds.), Saint Joseph.

  • Cardinaud, G., Rozière, E., Martinage, O., Loukili, A., Barnes-Davin, L., Paris, M., et al. (2021). Calcined clay – Limestone cements: Hydration processes with high and low-grade kaolinite clays. Construction and Building Materials, 277, 122271. https://doi.org/10.1016/j.conbuildmat.2021.122271

    Article  Google Scholar 

  • Córdoba, G. P., Zito, S. V., Sposito, R., Rahhal, V. F., Tironi, A., Thienel, C., et al. (2020a). Concretes with calcined clay and calcined shale: Workability, mechanical, and transport properties. Journal of Materials in Civil Engineering, 32(8), 1–11. https://doi.org/10.1061/(ASCE)MT.1943-5533.0003296

    Article  Google Scholar 

  • Córdoba, G. P., Zito, S. V., Tironi, A., Rahhal, V. F., & Irassar, E. F. (2020b). Durability of concrete containing calcined clays: Comparison of illite and low-grade kaolin. In S. Bishnoi (Ed.), Calcined clays for sustainable concrete, Proceedings of the 3rd international conference on calcined clays for sustainable concrete (pp. 631–640). RILEM Book. https://doi.org/10.1007/978-981-15-2806-4_70

    Chapter  Google Scholar 

  • Danner, T., Norden, G., & Justnes, H. (2018). Characterization of calcined raw clays suitable as supplementary cementitious materials. Applied Clay Science, 162, 391–402. https://doi.org/10.1016/j.clay.2018.06.030

    Article  Google Scholar 

  • Dapena, G. (1978). Study of the influence of weathering on the characteristics of the stone materials used in the public works project. The Polytechnic University of Madrid, Madrid, Spain.

    Google Scholar 

  • Dearman, W. R. (1974). Weathering classification in the characterization of rock for engineering purposes in British practice. Bulletin of the International Association of Engineering Geology, 14, 123–127. https://doi.org/10.1007/BF02634744

    Article  Google Scholar 

  • Dixit, A., Du, H., & Pang, S. D. (2021). Performance of mortar incorporating calcined marine clays with varying kaolinite content. Journal of Cleaner Production, 282, 124513. https://doi.org/10.1016/j.jclepro.2020.124513

    Article  Google Scholar 

  • Fernández, R., Martirena, F., & Scrivener, K. L. (2011). The origin of the pozzolanic activity of calcined clay minerals: A comparison between kaolinite, illite and montmorillonite. Cement and Concrete Research, 41(1), 113–122. https://doi.org/10.1016/j.cemconres.2010.09.013

    Article  Google Scholar 

  • Fernández, M., Alba, M. D., & Torres, R. M. (2013). Effects of thermal and mechanical treatments on montmorillonite homoionized with mono - and polyvalent cations: Insight into the surface and structural changes. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 423, 1–10. https://doi.org/10.1016/j.colsurfa.2013.01.040

    Article  Google Scholar 

  • García, E., & Suárez, M. (2003). Clays: properties and uses. Complutense University of Madrid.

    Google Scholar 

  • He, C., Osbaeck, B., & Makovicky, E. (1995). Pozzolanic reactions of six principal clay minerals: Activation, reactivity assessments and technological effects. Cement and Concrete Research, 25(8), 1691–1702. https://doi.org/10.1016/0008-8846(95)00165-4

    Article  Google Scholar 

  • Irassar, E. F., Bonavetti, V. L., Castellano, C. C., Trezza, M. A., Rahhal, V. F., Córdoba, G., et al. (2019). Calcined illite-chlorite shale as supplementary cementing material: Thermal treatment, grinding, color and pozzolanic activity. Applied Clay Science, 179, 105143. https://doi.org/10.1016/j.clay.2019.105143

    Article  Google Scholar 

  • Kakali, G., Perraki, T., Tsivilis, S., & Badogiannis, E. (2001). Thermal treatment of kaolin: The effect of mineralogy on pozzolanic activity. Applied Clay Science, 20, 73–80. https://doi.org/10.1016/S0169-1317(01)00040-0

    Article  Google Scholar 

  • Little, A. (1969). The engineering classification of residual tropical soils. In 7th International Conference of Soil Mechanics and Foundation Engineering (Ed.), Proceedings of the specialty session on the engineering properties of alteration soils (pp. 1-10). Mexico City.

  • Lothenbach, B., Scrivener, K., & Hooton, R. D. (2011). Supplementary cementitious materials. Cement and Concrete Research, 41(12), 1244–1256. https://doi.org/10.1016/j.cemconres.2010.12.001

    Article  Google Scholar 

  • Madejová, J. (2003). FTIR techniques in clay mineral studies. Vibrational Spectroscopy, 31(1), 1–10. https://doi.org/10.1016/s0924-2031(02)00065-6

    Article  Google Scholar 

  • Marchetti, G., Rahhal, V. F., Pavlík, Z., Pavlíková, M., & Irassar, E. F. (2020). Assessment of packing, flowability, hydration kinetics, and strength of blended cements with illitic calcined shale. Construction and Building Materials, 254, 119042. https://doi.org/10.1016/j.conbuildmat.2020.119042

    Article  Google Scholar 

  • Nesbitt, H. W., & Young, G. M. (1982). Early Proterozoic climates and plate motions inferred from major element chemistry of lutites. Nature, 299, 715–717. https://doi.org/10.1038/299715a0

    Article  Google Scholar 

  • Nesbitt, H. W., & Young, G. M. (1984). Prediction of some weathering trends of plutonic and volcanic rocks based on thermodynamic and kinetic considerations. Geochimica et Cosmochimica Acta, 48(7), 1523–1534. https://doi.org/10.1016/0016-7037(84)90408-3

    Article  Google Scholar 

  • Nesbitt, H. W., & Young, G. M. (1989). Formation and diagenesis of weathering profiles. Journal of Geology, 97(2), 129–147. https://doi.org/10.1086/629290

    Article  Google Scholar 

  • Plouffe, A., McClenaghan, M. B., Paulen, R. C., McMartin, I., Campbell, J. E., & Spirito, W. A. (2013). Quality assurance and quality control measures applied to indicator mineral studies at the Geological Survey of Canada. In R. C. Paulen & M. B. McClenaghan (Eds.), New frontiers for exploration in glaciated terrain, open file 7374 (pp. 13–20). Geologic Survey of Canada. https://doi.org/10.4095/292679

    Chapter  Google Scholar 

  • Rakhimova, N. R., Rakhimov, R. Z., Bikmukhametov, A. R., Morozov, V. P., Eskin, A. A., Lygina, T. Z., et al. (2020). Role of clay minerals content and calcite in alkali activation of low-grade multimineral clays. Journal of Materials in Civil Engineering, 32(8), 04020198. https://doi.org/10.1061/(asce)mt.1943-5533.0003255

    Article  Google Scholar 

  • Rodríguez, C., & Tobón, J. I. (2020). Influence of calcined clay/limestone, sulfate and clinker proportions on cement performance. Construction and Building Materials, 251, 119050. https://doi.org/10.1016/j.conbuildmat.2020.119050

    Article  Google Scholar 

  • Rodríguez, J., Frías, M., & Tobón, J. I. (2021). Eco-efficient cement based on activated coal washing rejects with low content of kaolinite. Construction and Building Materials, 274, 122118. https://doi.org/10.1016/j.conbuildmat.2020.122118

    Article  Google Scholar 

  • Roy, S., Chatterjee, A., & Aiyer, H. (2020). Effect of mineralogy and temperature treatment on the pozzolanic activity of Indian clays. Materials Research Innovations, 24(1), 18–27. https://doi.org/10.1080/14328917.2018.1546794

    Article  Google Scholar 

  • Samet, B., Mnif, T., & Chaabouni, M. (2007). Use of a kaolinitic clay as a pozzolanic material for cements: Formulation of blended cement. Cement and Concrete Composites, 29(10), 741–749. https://doi.org/10.1016/j.cemconcomp.2007.04.012

    Article  Google Scholar 

  • Schmid, R., Fettes, D., Harte, B., Davis, E., Desmons, J., Meyer-Marsilius, J., & Siivola, J. (2004). A systematic nomenclature for metamorphic rocks: 1. How to name a metamorphic rock. Resource document. Subcommission on the systematics of metamorphic rocks (SCMR).

  • Scrivener, K. (2014). Options for the future of cement. Indian Concrete Journal, 88(7), 11–21.

    Google Scholar 

  • Scrivener, K., Martirena, F., Bishnoi, S., & Maity, S. (2018). Calcined clay limestone cements (LC^3). Cement and Concrete Research, 114, 49–56. https://doi.org/10.1016/j.cemconres.2017.08.017

    Article  Google Scholar 

  • Shvarzman, A., Kovler, K., Schamban, I., Grader, G. S., & Shter, G. E. (2002). Influence of chemical and phase composition of mineral admixtures on their pozzolanic activity. Advances in Cement Research, 14(1), 35–41. https://doi.org/10.1680/adcr.2002.14.1.35

    Article  Google Scholar 

  • Sposito, R., Maier, M., Beuntner, N., & Thienel, K. (2022). Physical and mineralogical properties of calcined common clays as SCM and their impact on flow resistance and demand for superplasticizer. Cement and Concrete Research, 154, 106743. https://doi.org/10.1016/j.cemconres.2022.106743

    Article  Google Scholar 

  • Sunitrová, I., & Trník, A. (2018). DSC and TGA of a kaolin-based ceramics with zeolite addition during heating up to 1100°C. AIP Conference Proceedings, 1988, 020046. https://doi.org/10.1063/1.5047640

    Article  Google Scholar 

  • Tironi, A. (2013). Low energy cementitious materials. Thermal Activation clays, the relationship between structure and pozzolanic activity. PhD thesis, National University of La Plata, La Plata, Buenos Aires, Argentina.

  • Tironi, A., Trezza, M. A., Scian, A. N., & Irassar, E. F. (2012). Kaolinitic calcined clays: Factors affecting its performance as pozzolans. Construction and Building Materials, 28(1), 276–281. https://doi.org/10.1016/j.conbuildmat.2011.08.064

    Article  Google Scholar 

  • Tironi, A., Castellano, C. C., Bonavetti, V. L., Trezza, M. A., Scian, A. N., & Irassar, E. F. (2014a). Kaolinitic calcined clays-Portland cement system: Hydration and properties. Construction and Building Materials, 64, 215–221. https://doi.org/10.1016/j.conbuildmat.2014.04.065

    Article  Google Scholar 

  • Tironi, A., Trezza, M. A., Scian, A. N., & Irassar, E. F. (2014b). Potential use of Argentine kaolinitic clays as pozzolanic material. Applied Clay Science, 101, 468–476. https://doi.org/10.1016/j.clay.2014.09.009

    Article  Google Scholar 

  • USGS (2019). Drilling Methods Used by the Western Region Research Drilling Program. United States Geological Survey.

  • Vásquez, O., Carmona, S., & Tobón, J. I. (2020). Cement production with pozzolans from residual tropical soils formed from Paragneiss with a high silicon oxide content. Dyna (Colombia), 87(213), 69–74. 10.15446/dyna.v87n213.83208.

  • Yanguatin, H., Tobón, J., & Ramírez, J. (2017). Pozzolanic reactivity of kaolinitic clays, a review. Revista Ingeniería de construcción, 32(2), 13–24.

  • Yanguatin, H., Ramírez, J. H., Tironi, A., & Tobón, J. I. (2019). Effect of thermal treatment on pozzolanic activity of excavated waste clays. Construction and Building Materials, 211, 814–823. https://doi.org/10.1016/j.conbuildmat.2019.03.300

    Article  Google Scholar 

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Acknowledgments

The authors are grateful to the Cement and Building Materials Research Group (CEMATCO) of the School of Mines and the Department of Materials and Minerals of Universidad Nacional de Colombia.

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The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

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Correspondence to Oscar O. Vásquez-Torres.

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Vásquez-Torres, O.O., Cabrera-Poloche, F.D. & Tobón, J.I. Performance of Low-Grade Calcined Clays as Supplementary Cementitious Material in Relation to their Geological Characteristics. Clays Clay Miner. 70, 233–251 (2022). https://doi.org/10.1007/s42860-022-00184-7

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