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In this paper, we demonstrate the value of 1 H NMR relaxometry for studying the hydration of clinker-reduced, climate-friendly cementitious binders. Our study includes white cement (WC), ordinary Portland cement (OPC), and samples incorporating reactive agro-waste based ashes and non-reactive biochars as supplementary cementitous materials (SCM). NMR measurements were performed over a period of up to 120 h during hydration with an echo time of 50 μ s and a relatively large sample size of 20 mL. The results were compared to heat flow calorimetry (HFC) data, and a detailed comparison with literature data was performed for pure OPC and WC. The results show that time-resolved NMR measurements, especially the analysis of individual NMR signal components assigned to defined 1 H reservoirs, are effective for studying hydration processes. They offer insights into the evolution of the microstrucure and specific chemical phases. NMR provides valuable information and serves as a good complement to HFC. The comparison with data obtained with shorter echo times (40 μs or around 15–45 μs with solid echo sequence) on much smaller samples showed almost identical developments with respect to the T2 distributions. For the SCM samples, NMR results indicated partially accelerated hydration processes compared to classical OPC hydration. One SCM sample acted as a highly reactive pozzolan, showing a similar hydration process to OPC with the strongest effect observed when superplasticizer was added.
Adding biochar delayed C-S-H gel pore formation but significantly increased capillary pores and even free water, likely due to the sponge-like structure.
The construction sector accounts for 40% of global carbon emissions, and its impact is set to rise as growing populations drive increased construction activity, particularly in the Global South. In Africa, where cement is expensive and urban growth is rapid, innovative, locally tailored solutions are urgently needed. To address this environmental challenge, a common approach is to use limestone-calcined clay cement (LC3), which allows for approximately 50% clinker reduction with equivalent performance to OPC. However, LC3 often presents challenges in terms of fresh concrete properties due to its influence on rheological properties. This paper proposes the use of gum Arabic (GA), a polysaccharide biomass abundant in Africa, as a rheology modifying admixture. These local admixtures would provide access to chemical admixtures for a wider range of concrete users, including the informal sector, and create local value chains while minimising dependence on global supply streams. Rheometer, 1H nuclear magnetic resonance (1H NMR) and heat flow calorimetry (HFC) techniques were used to understand the influence of GA on both OPC and LC3 systems by monitoring their early hydration. Rheological results reveal that GA affects the fresh paste rheology of OPC and LC3 systems differently, requiring different dosages to achieve optimal performance. Heat flow and NMR analyses further confirm that GA retards the hydration reactions in both systems.
The use of biochar as a supplementary cementitious material is proposed to reduce the global greenhouse gas emissions. Since biochar is non-reactive, has a low density and complex porosity, its incorporation into cementitious materials results in microstructural changes and consequently affects the mechanical response. This work advances the mechanical response understanding of Portland cement composites with 0, 5, and 25 volume percent (vol%) of cement replaced with biochar by using in-situ computed tomography, correlating with the microstructural changes analyzed by HFC, gas sorption, MIP, gas sorption, and NMR. The results highlight the influence of the mesoscale structure on mechanical responses and relate the lack of loss of mechanical strength at 5 vol% replacement to the compensation of decreasing larger pores with biochar addition. At 25 vol% replacement, the amount of weakened zones in the paste due to biochar overcompensates the positive effect of the reduction in larger pores, resulting in a loss of mechanical properties. Hence, small amounts of biochar can enhance the microstructure, but the reduction of the carbon footprint is limited.
The use of biochar as a concrete constituent has been proposed to reduce the massive carbon footprint of concrete. Due to the low density and complex porosity of biochar, microstructural analysis of Portland cement-biochar composites is challenging.
This causes challenges to the improvement of the micro-scale understanding of biochar composite behavior. This work advances the microstructural understanding of Portland cement composites with 0, 5, and 25 volume percent (vol%) of cement replaced with wood biochar by applying common characterization techniques of mercury intrusion porosimetry (MIP), gas sorption, scanning electron microscopy, and isothermal heat flow calorimetry (HFC) in conjunction with 1H nuclear magnetic resonance (NMR) and micro-X-ray computed tomography (XCT) analysis techniques. The combination of these techniques allows a multi-scale investigation of the effect of biochar on the microstructure of cement paste. NMR and XCT techniques allow the observation and quantification of the pore space. HFC and MIP confirmed that biochar absorbs moisture and reduces the effective water-cement ratio. Gas sorption, MIP, and NMR shows that 5 vol% replacement does not significantly affect the gel and capillary pore structures. Results from XCT (supported by MIP and NMR) show that biochar can reduce the formation of larger pores.
Importantly, XCT results suggest that biochar can act as a flaw in the microstructure which could explain reductions in the mechanical properties. Overall, the mechanical properties already analyzed in the literature are consistent with the microstructural changes observed, and these results highlight the need to carefully tailor the volume fraction of biochar to control its effect on the paste microstructure.
In this paper, we demonstrate the value of 1H NMR relaxometry for studying the hydration of clinker-reduced, more climate-friendly cementitious binders. The results were obtained on typical CEM I cements and sister samples containing two different reactive agricultural ashes as well as non-reactive biochars as supplementary cementitious materials. The findings prove that time-resolved NMR measurements provide valuable additional information when combined with classical heat flow calorimetry.
The global demand for concrete is growing, and with it, its carbon footprint. Current literature proposes biochar, a product of pyrolysis, as a possible car-bon sink to reduce the carbon footprint of concrete. This work investigates the microstructure of Portland cement pastes with 0%, 5%, and 25% of the cement replaced with wood biochar, since this should influence its macro-scopic mechanical properties. MIP, gas sorption, NMR, and µ-CT were used to analyze the pore space of the three materials. The combination of these methods, each with different resolution, enables a multi-scale investigation of biochar impact on the microstructure of cement pastes. NMR confirmed that biochar can absorb moisture and, thus, reduces the effective water-to-cement ratio. MIP and gas sorption results show 0% and 5% volume re-placement have similar gel pore structure. The results from µ-CT investiga-tions suggest that biochar may reduce the formation of larger pores. The in-clusion of non-reactive porous particles such as biochar increase the porosity of the material and should act as a weakness in terms of mechanical proper-ties. Overall, this study highlights the need to carefully tailor replacement rates to control the impact of biochar on the microstructure concrete mixtures and sees a strong need for further studies on mechanical properties.
This study addresses biochar as a potential carbon-sequestering filler in cement and examines its effect on mechanical properties using X-ray computed tomography (XCT) and digital volume correlation (DVC). DVC was reliably used to measure global displacement and has proven to be an effective method for correcting displacement data obtained from mechanical tests conducted without traditional instrumentation, such as extensometer. This made it possible to measure strain and Young’s modulus accurately. The results demonstrate that while 5 vol% biochar replacement had minimal effect on mechanical properties, a 25 vol% biochar replacement caused a 35 % reduction in Young’s modulus and 40 % reduction in the ultimate compressive strength. Additionally, DVC detected strain concentrations and predicted material failure locations even when cracks could not be quantified using XCT alone. Moreover, the study reveals that biochar particles, due to their sharp geometry, increase internal shear strain during uniaxial compression, unlike round phases such as pores.
Real-time monitoring of structural build-up is critical for robust 3D concrete printing (3DCP). We evaluate electromechanical impedance (EMI) sensing with embedded piezoelectric (PZT) sensors to track early-age structuration of cementitious binders, a key phenomenon for 3DCP. Cement pastes (CEM I 42.5 R) spanning water-to-cement ratios w/c = 0.32, 0.36, 0.40 and a phosphate-retarded paste were cast with embedded sensors. Electrical impedance (EI) measurements were recorded from casting to 4 h for the w/c series (0–7 h for the retarded mix) and were normalized to each sensor’s in-air baseline. The fundamental resonance was very sensitive to the surrounding medium: immediately after embedding, the conductance peak decreased and the resonance shifted to lower frequency, followed by continued attenuation during the nominal dormant period. Over the hydration window studied, peak-conductance amplitude was more sensitive to microstructural changes than resonance-frequency shift, and this amplitude-based metric correlated with reference measurements: small-amplitude oscillatory shear (SAOS) rheometry and Vicat penetration. The rate of change in peak-conductance amplitude ranked with composition (WC32 > WC36 > WC40). The retarded mix showed an unusual early build-up signature that preceded the hydration-driven percolation knee seen in rheology, which was reflected in the conductance trends. The mapping between shear modulus and conductance-derived features was nonlinear. EI spectrum responded from the time of casting, providing the earliest actionable indicator for process control. Overall, this preliminary study with standard cement pastes indicates that the EMI sensing offers a sensitive, embedded, and physically interpretable route to in-situ monitoring of fresh-state evolution, with potential to define practical setpoints (for example, interlayer wait times), while Vicat and rheology serve as benchmarks and calibration companions.
