Abstract
The drive towards improving the properties of cement composite thus making it eco-friendly, sustainable, and durable, has been the focus of the construction industry. Kaolin is one of the pozzolans that have been investigated in recent times, but its reactivity is influenced by its source. In addition, the problem of homogenous mixing onsite and early strength development of pozzolana blended cement are evident. This research focused on the strength and microstructural properties of factory-produced metakaolin blended cement incorporated with green nanosilica. Kaolin samples were obtained from three locations and calcinated at 700 ℃ for 1 h. Metakaolin was interground with 10% Portland Limestone Cement (PLC) clinker at the factory. Binder-sand ratio (1:3) with a water-binder ratio of 0.5 was adopted for batching the mortar. Nanosilica was added to the mortar at: 1, 2, 3, 4, and 5%, respectively. Prisms of 40 × 40 × 160 mm were cast and cured for 3, 7, 14, 28, 56, 90, 180, 270, and 365 days, respectively. The flexural and compressive strengths of prisms including the water absorption of cubes were evaluated. 10% MK addition enhanced the mechanical properties of the mortar with MK C having the highest enhancement. Incorporation of 1% nanosilica enhanced strengths at early and later ages, as well as refinement in the pores of the mortar with increasing nanosilica.
Article Highlights
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Intergrinding metakaolin with Portland Limestone clinker at the factory to produce metakaolin blended cement.
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Sourcing of Kaolin from three different locations as against previous work.
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The nanosilica used was synthesized using extracts of cola pod nitida.
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1 Introduction
The behaviour of mortar and concrete composites depends on the characteristics of the binding material as it plays a significant role in making the constituents to form a compact whole [1]. The production of the conventional binder (Portland Limestone Cement) is energy intensive and associated with the release of carbon dioxide into the atmosphere, which in turn has tendency of deleting the ozone layer. Thus, resulting into warming of the globe [2]. There is a need to explore the application of some materials with a tendency to exhibit supplementary cementitious properties that are friendly to the ecosystem through a reduction in the emission of carbon dioxide and other related greenhouse gases with corresponding reduction in cost of production of composites [1, 3]. These materials could be agricultural residues, industrial by-products or naturally occurring. Amongst are fly ash, rice husk ash, guinea corn ash, wood ash, neem seed ash, bone ash, silica fume, activated alum sludge, and metakaolin (MK). The addition of these Supplementary Cementitious Materials (SCMs) to PLC could be by intergrinding or onsite mixing to produce blended cements. Numerous works have been done on the use of industrial wastes and agricultural residues. It is very pertinent to focus on the applications of naturally occurring clay as a partial replacement of cement in the production of concrete composites. Metakaolin (MK) being a new category of SCM, has the advantages of improving the properties of concrete composite, and solving environmental issues on the premise of reducing the emission of carbon dioxide [4, 5].
MK is alumino silicate in nature, which is being produced as a result of the thermal transformation of kaolin clay between 700 and 850 °C. The calcination parameters (temperature and time) have significant effects on the pozzolanicity of the MK. A temperature of 700 °C and a duration of 1 h have been recommended to produce MK with a good reactivity tendency [4, 6,7,8]. Also, the source or location where the kaolin is obtained has an influence on the chemical compositions as well as the structural arrangements of its constituting minerals. Furthermore, this determines the characteristics or reactivity of the kaolin [9]. MK has been found to possess unique properties as compared to other pozzolans because it involves the dehydroxylation of naturally occurring kaolin clay as well as having the following attributes: enhancement in the hydration reaction of cement, dilution effects, improvement in workability, and enhancement in an early strength development of mortar or concrete [10,11,12].
Nanomaterials are materials having a particle size in nanometres. These materials have been reported to enhance the physicomechanical properties of cement composites at elevated temperatures [3]. The fine nature and their sizes on the nanoscale enhance the properties of mortar and concrete when incorporated into the matrix. This is being initiated during the hydration of the cement [13, 14]. The addition of nanosilica (NS) to mortar and concrete has been reported to improve the properties of the composites both in fresh and hardened states [13, 21]. Thereafter, the Ultraviolet Visible (UV–VIS) spectrometry of the cola pod extract and nanosilica was investigated to determine the absorption of the particles. Also, an energy dispersive X- ray (EDX) of the nanosilica was performed to enable the determination of the elemental composition of the synthesized nanosilica. Sand-binder ratio 1:3 with water-binder ratio 0.5 was adopted in accordance with the work of other researchers elsewhere [22,23,24,25]. Also, these were adopted to produce MK blended cement mortar with nanosilica at levels of 1, 2 3, 4 and 5% by weight of the binder. Cement mortar was cast in prism size of 40 × 40 × 160 mm, cast in triplicates, and cured in water for 3, 7, 14, 28, 56, 90, 180, 270, and 365 days, respectively. The flexural strength was conducted on the prism with the application of load at the third point on the prism until failure occurred as shown in Fig. 3a. Thereafter, compressive strength was performed on the half of the prism obtained after flexural strength test as presented in Fig. 3b. The flexural and compressive strengths were performed using Toni Technik compressive and flexural strength model: 1544 in accordance with BS EN 196 [26]. Using Design Expert Software version 13, an analysis of their data was conducted to determine the relationship between flexural and compressive strength.
3 Results and discussion
3.1 UV–VIS spectroscopy of cola pod extract and nanosilica
The UV–VIS spectra for cola pod nitida extract and synthesized nanosilica are presented in Figs. 4 and 5, respectively. The peak absorption of 1.124 Abs for the extract occurred at a wavelength of 298 nm and that of the nanosilica with absorbance of 2.292 occurred at a wavelength of 236 nm. The value for the wavelength as obtained in the case of the extract could be attributed to the double bond system contained in the cola pod extract as reported by Bisiriyu [27]. However, the wavelength of 236 nm for synthesized nanosilica was in close agreement with the value of 235 nm where a sol–gel method of synthesizing nanosilica was adopted [28] and greater than 200, 204 and 228.3 nm as reported by Al-Abboodi [29], Engku [30], Qasim [31], respectively.
3.2 EDX of nanosilica
The elemental composition of the synthesized nanosilica is presented as shown in Fig. 6. The spectrum revealed silicon as the dominating element amongst others with a relative abundance of 65.2%. The value was found to be greater than 61. 28% as obtained in the work of Behnia [32] where nanosilica was synthesized using sulphuric acid and ethanol in combination with a surfactant calcined at halved temperature of 1000 °C.
3.3 Flexural strength of metakaolin blended cement mortar containing nanosilica
Flexural strength for PLC and MK blended cement mortar sourced from different locations infused with nanosilica is presented in Figs. 7, 8, 9. These figures show that flexural strength of 10% MK blended cement surpassed that of the PLC at early and later ages. This agrees with the work of Regina [33], Menshaz [34]. The addition of nanosilica to the blended cement mortar up to a level of 1% was observed enhance the flexural strength at both early and later curing ages. This agrees as reported in other research, where 1% nanosilica addition to cement mortar and concrete gave maximum flexural strength [18, 19, 35, 36]. The flexural strength was observed to reduce as the percentage of nanosilica increased from 2 to 5%. The reduction in strength may be due to the formation of excessive nucleation sites outweighing the atoms reacting together. In addition, the problem of adequate dispersion of the nanosilica could lead its agglomeration [37, 38]. Figure 9 shows the flexural strength of MK blended cement obtained from sample C, which surpassed that of Figs. 6 and 7 (representatives of samples A and B, respectively). This is an indication that the source of kaolin clay had an influence on the bending strength of MK blended cement mortar.
3.4 Compressive strength of metakaolin blended cement mortar containing nanosilica
Figures 10, 11, 12 show the compressive strength of PLC, MK blended cement with and without nanosilica for samples A, B and C, respectively. These Figures revealed the compressive strength for PLC at the end of 365 days to be 65. 75 N/mm2. MK blended cement mortar at same curing ages ranged 67.98–70.13 N/mm2. The result showed enhancement in compressive strength of MK blended cement mortar as compared to that of PLC. This agrees with the findings of Menshaz [34], Alonge [39], Naresh [40]. The incorporation of nanosilica to MK blended cement mortar was observed to initially increase the compressive strength and decreased with subsequent addition of nanosilica; 1% nanosilica given the maximum compressive strength. This is as reported elsewhere [18, 19, 35, 36]. The compressive strength was observed to decrease as the percentage of nanosilica was increased from 2 to 5%. The reduction may be because of excessive nucleation site formation and problem of dispersion of more content of nanosilica [37, 38]. The trend of result as obtained in this work is in contrary to the findings of Ltifi [41] where the influence of nanosilica was examined on the behaviour of PLC mortar. It was observed that the compressive strength increased as the percentage of nanosilica was increased between 3 and 10%. This may be because the binder used was PLC alone and not pozzolana blended cement. Figures 10, 11, 12 revealed the compressive strengths of MK blended cement mortar obtained from different locations with addition of nanosilica. Figure 12 showed strength of sample C which surpassed Figs. 10 and 11, samples A and B, respectively. This is an indication of influence of location of MK on the strength of the blended cement mortar.
3.5 Relationship between flexural and compressive strength of metakaolin blended cement mortar with nanosilica
The flexural and compressive strengths are parameters that determine the viability and behavioural pattern of a material under loading or while in use. The need to establish the relationship between the two dependent variables is important as it enhances the prediction or determination of one unknown parameter if the other is evaluated or determined.
3.5.1 Overview of the experimental setup
Using the response surface methodology of central composite design on Design expert software version 13 (DOEv13) [42], the experimental design was completed. Two selected parameters were added to the CCD's empirical domain in order to generate experimental sets. With no blocks and responses in the form of flexural and compressive strength, the polynomial (fifth) design model was used. The two parameters that were chosen considering their levels’ ranges, the design generated fifty-seven (57) runs; the findings showed that no performance changes were applied to the responses as presented in Table 3.
3.5.2 Responses to experimental details
The responses' extreme and minimal frequencies, along with the corresponding runs for each factor, are summarized in Table 4. It was found that the anticipated ranges for compressive and flexural strength were 23.812 to 76.731 N/mm2 and 6.624 to 15.939 N/mm2, respectively.
3.5.3 Overview and modification parameters for the model
Table 5 shows the model overview and modification parameters for the responses of compressive and flexural strength. The standard deviation displays the error, or degree of variation, between the experimental and true values. They were in the range of 0.297 and 0.432 for both responses. They had expected (r2) values ranging from 0.933 to 0.952, whereas their fitted (R2) values were between 0.9575 and 0.9744. According to [42, 43], all expected (r2) values agreed with the fitted (R2) values for both responses because their differences were less than 0.2.
The range of values for the signal-to-noise ratio measured with tolerable accuracy is 28.758–42.828. These showed that both models had sufficient signals to explore the design space, as evidenced by their appropriate precision ratings exceeding 4.0. Additionally, all of the models' p values were less than 0.05 (p < 0.05), and their F values (i.e. p < 0.0001), demonstrating their importance with no complacency [42, 43].
3.5.4 ANOVA (variance’s analysis)
The summary of surface polynomial (fifth) response models' Analysis of Variance (ANOVA) results of flexural and compressive strengths is displayed in Table 6. The model was significant, as indicated by its F-value of 107.47. There is likelihood of noise producing high Model F at about 0.01%. If the value of P (i.e., 95% confidence interval) was less than 0.05, model parameters were considered highly meaningful; if the value was more than 0.10, the parameters were not meaningful. The model terms become more important when the absolute F-value increases and the P-value decreases. In this instance, major important model parameters were A, B, A2, B2, A2B, A3, B3, A3B, A4, A4B, A5, and B5. Other model parameters needed to preserve the hierarchy [42, 43].
3.5.5 Equations of the model
Equations (1) and (2) are the equations for regression that were used to forecast the responses i.e. the flexural and compressive strength (ultimate experimental models in the form of coded components). A negative sign before the words denotes an opposing impact, whereas a plus sign denotes a cooperative impact on the observed response. B is the curing age (days), and A is the MK C.
3.5.6 Model charts
Figure 13 shows the relationship between the flexural and compressive strength of MK blended cement mortar infused with nanosilica at a level of 1%. The curve gave a coefficient of determination (R2) value of between 0.945 and 0.955 with a polynomial geometry adopted as the best curve fitting. The responses' anticipated and experimental values agreed quite well, with the greatest r2 value being 0.952. There was no difference between the true and expected values where flexural and compressive strength values met. Nonetheless, the values were either positive (flexural > compressive strength), indicating that the true values exceeded what was expected, or negative, indicating that the true values were lower or vice versa. These charts demonstrated good residual normality. The correlation between the true and expected values of the responses was supported by the r2 values in Table 5.
This geometry is in line with the findings of Zhang [44]. However, the value of (R2) obtained in the work of Shodolapo [45] was found to be 0.8037 where quadratic pattern of curve was adopted. The discrepancy in value may be attributed to the quadratic pattern as against the polynomial or cubic curve fittings adopted. However, the quadratic curve showed a very good correlation between the flexural and compressive strength as the value approaches unity [46]. The value of coefficient of determination obtained in this work is close agreement with 0.989 as obtained in the work of Yusuf [47] where an appropriate relationship between flexural and compressive strength of palm kernel shell concrete was investigated. The work concluded a polynomial curve fitting to be the best relationship.
Figure 14 displays the contour and 3D response area graphs for the flexural and compressive strength responses as functions of the MK sourced at location C and Curing age. The determined response surface forecasts were used to verify the models. The hot (main) reaction zone made by the graphs encompassed all the forecasts. The figure's red colour denotes the primary reaction zone, green denotes a potential reaction zone (meaning that reaction can occur there even in the presence of impurities), and blue denotes a cold reaction zone (meaning that though there may be a reaction in this area, it is not very likely). The models' four edges natures show the important role of both aspects in the processes. Equations (1) and (2) show how the graph types reaffirmed the models' polynomial structure. Figures 13 and 14 showed how compressive strength increases with flexural strength and vice versa.
3.5.7 Optimization
According to Table 7, the optimal results for flexural and compressive strength was 15.939 and 76.731 N/mm2, respectively. Maximum compressive strength and maximum flexural strength were obtained with these results. Their standard error was sufficiently small, ranging from 0.282 to 1.943%. Given that it was less than 5%, the results were good.
3.6 Water absorption of metakaolin blended cement mortar containing nanosilica
The water absorption of blended cement obtained from different kaolin locations with addition of 5% nanosilica at the end of 28 days for samples A, B, and C are 1.01, 1.20 and 1.03% respectively as presented in Fig. 15. These values were observed to be lower than 1.72, 1.65, and 1.56% MK blended cement of samples A, B, and C, respectively. Also, the water absorption for PLC at the same curing age was found to be 1.98%. The graph revealed a reduction in water absorption as the percentage of nanosilica increased. This may be attributed to the reduction in the pores of the hardened mortar which is an indication of the pore refinement tendency exhibited by nanosilica [48, 49].
3.7 Microstructure of OPC and metakaolin blended cement
Figure 16 shows the SEM micrograph of OPC and that of MK blended cements. The MK blended cement shows micrograph that is plate like in nature. This agrees with the findings as obtained elsewhere [50,51,52]. Figure 16c and d show blended cement with predominance of plate like structure. This is an indication of high amorphous tendency exhibited by the duo when compared to Fig. 16a. This may be attributed to the effect of the source of kaolin on the characteristics of the binder.
3.8 Microstructure of metakaolin blended cement mortar containing nanosilica
The pores in the MK blended cement mortar in the hardened state were observed to reduce with addition of 1% nanosilica as presented in Fig. 17. The micrographs showed denser medium with C–S–H bonding enhanced due to the incorporation of nanosilica as compared with that of MK blended cement shown in Fig. 16. The refinement exhibited is in agreement with some previous work [33, 53].
4 Conclusion
At the end of this research, the following conclusions were drawn:
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Intergrinding of 10% MK with PLC shows enhancement in flexural and compressive strengths as compared to the conventional PLC binder.
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The source of kaolin clay influenced the reactivity of MK, and consequently, the properties of MK blended cement.
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The compressive and flexural strengths of MK blended cement mortar were enhanced at a low percentage of nanosilica addition.
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The high wavelength recorded in the synthesized nanosilica could be attributed to the conjugate double bond exhibited by the cola pod extract.
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The addition of nanosilica enhanced the pore fineness of hardened metakaolin blended cement mortar.
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Addition of nanosilica reduced the water absorption of metakaolin blended cement mortar with 5% nanosilica having the least water absorption.
Data availability
All data used in this manuscript do not involve human/living organisms and were results of laboratory investigations carried out on the application of metakaolin blended cement. The procedures to achieving these results have been extensively described under the methodology. No data were sourced online or replicated from previous studies; all information is primary and, on this note, no available link to any data. In addition, appropriates references have been duly cited in the work to corroborate the findings of previous work done.
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Acknowledgements
The authors acknowledged the supports members of LAUTECH Nano+Research group, LAUTECH, Ogbomoso, Nigeria and Technical staff in the Laboratory of the West African Portland Cement, Lafarge, Sagamu, Ogun State, Nigeria.
Funding
Open access funding provided by University of South Africa.
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AAR: Conceptualization, Supervision, Methodology, Investigation, Writing- review & editing, Validation. RA: Conceptualization, Data curation, Formal analysis, Funding acquisition, Investigation, Methodology, Resources, Visualization, Writing- original draft. BDI: Formal analysis, writing- review & editing. EAA: Formal analysis, writing- review & editing. The authors acknowledged the supports members of LAUTECH Nano+Research group, LAUTECH, Ogbomoso, Nigeria and Technical staff in the Laboratory of the West African Portland Cement, Lafarge, Sagamu, Ogun State, Nigeria.
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Raheem, A.A., Abdulwahab, R., Ikotun, B.D. et al. Evaluation of the strength performance and microstructural properties of different based metakaolin blended cements containing greenly synthesized nanosilica. Discov Appl Sci 6, 239 (2024). https://doi.org/10.1007/s42452-024-05890-6
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DOI: https://doi.org/10.1007/s42452-024-05890-6