Microstructural Evolution and Durability of Fly Ash–Bentonite Cementitious Composites Under Freeze–Thaw and Wet–Dry Cycling in Sulfate Environments: An Interpretable Machine Learning Approach

Sulfate-bearing cyclic environments induce coupled degradation of hydration gels and pore structure, but the differences between freeze–thaw and wet–dry deterioration remain unclear. Nine fly ash–bentonite cementitious composites with fly ash-to-cement ratios of 1.2, 1.8, and 2.4 and bentonite contents of 0%, 3%, and 6% were exposed to water, 10% Na2SO4, and 10% MgSO4 for up to 150 cycles. Macroscopic durability was evaluated using the squared ultrasonic pulse-velocity index (plotted as apparent RDEM), compressive-strength retention, and peak-stress retention; hydration products and pore evolution were characterized by X-ray diffraction, scanning electron microscopy, and low-field nuclear magnetic resonance. Freeze–thaw cycling was mainly associated with physical cracking and a redistribution toward longer-T2 water-accessible relaxation components, whereas wet–dry cycling intensified salt crystallization and sulfate-product accumulation. Sodium sulfate exposure was associated with stronger ettringite and gypsum diffraction peaks, whereas magnesium sulfate exposure showed a stronger gypsum peak and a weaker portlandite peak. Among the tested complete formulations, moderate fly ash contents and low bentonite dosages (with corresponding water-reducer adjustments) provided the most balanced resistance, whereas FA/C = 2.4 with 6% bentonite generally deteriorated more rapidly. Based on pooled out-of-fold predictions, support vector regression performed best for the apparent RDEM indicator (R2 = 0.929), while random forest gave the highest accuracy for compressive-strength retention (R2 = 0.937) and peak-stress retention (R2 = 0.994); the first two targets had 378 condition records each and peak stress had 216 author-confirmed numerical values. In leave-one-mixture-out sensitivity analysis, the corresponding pooled R2 values were 0.897, 0.942, and 0.992, respectively; this analysis assesses interpolation to an unobserved combination within the tested 3 × 3 composition grid, not extrapolation beyond its factor levels. Recomputed grouped SHAP attribution identified cycle count as the leading input for apparent RDEM (44.94% of relative mean absolute attribution), while the exposure-regime input dominated strength retention (53.36%) and peak-stress retention (56.65%); cycle count × regime was the strongest pairwise interaction in both mechanical targets. At limit states of 60% RDEM and 75% compressive-strength retention, the predicted durability thresholds ranged from 17 to more than 150 cycles, with RDEM governing most cases. The proposed framework pairs crystalline-phase and pore-structure observations with interpretable durability prediction within the tested cyclic sulfate environments. These are exploratory laboratory-cycle thresholds. A 300-resample trajectory bootstrap quantified model-refit variation; neither the thresholds nor their intervals are calibrated to field service time.

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Journal
Gels
Published
2026-10-29
DOI
https://doi.org/10.3390/gels12110988
Primary Topic
Concrete and Cement Materials Research
Type
article
Field-Weighted Citation Impact
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article

Microstructural Evolution and Durability of Fly Ash–Bentonite Cementitious Composites Under Freeze–Thaw and Wet–Dry Cycling in Sulfate Environments: An Interpretable Machine Learning Approach

Nan Zhao, Chao Liu, Chao Zhu
1 links
Gels
Concrete and Cement Materials Research
article

Microstructural Evolution and Durability of Fly Ash–Bentonite Cementitious Composites Under Freeze–Thaw and Wet–Dry Cycling in Sulfate Environments: An Interpretable Machine Learning Approach

Nan Zhao, Chao Liu, Chao Zhu
article en

Abstract

Sulfate-bearing cyclic environments induce coupled degradation of hydration gels and pore structure, but the differences between freeze–thaw and wet–dry deterioration remain unclear. Nine fly ash–bentonite cementitious composites with fly ash-to-cement ratios of 1.2, 1.8, and 2.4 and bentonite contents of 0%, 3%, and 6% were exposed to water, 10% Na2SO4, and 10% MgSO4 for up to 150 cycles. Macroscopic durability was evaluated using the squared ultrasonic pulse-velocity index (plotted as apparent RDEM), compressive-strength retention, and peak-stress retention; hydration products and pore evolution were characterized by X-ray diffraction, scanning electron microscopy, and low-field nuclear magnetic resonance. Freeze–thaw cycling was mainly associated with physical cracking and a redistribution toward longer-T2 water-accessible relaxation components, whereas wet–dry cycling intensified salt crystallization and sulfate-product accumulation. Sodium sulfate exposure was associated with stronger ettringite and gypsum diffraction peaks, whereas magnesium sulfate exposure showed a stronger gypsum peak and a weaker portlandite peak. Among the tested complete formulations, moderate fly ash contents and low bentonite dosages (with corresponding water-reducer adjustments) provided the most balanced resistance, whereas FA/C = 2.4 with 6% bentonite generally deteriorated more rapidly. Based on pooled out-of-fold predictions, support vector regression performed best for the apparent RDEM indicator (R2 = 0.929), while random forest gave the highest accuracy for compressive-strength retention (R2 = 0.937) and peak-stress retention (R2 = 0.994); the first two targets had 378 condition records each and peak stress had 216 author-confirmed numerical values. In leave-one-mixture-out sensitivity analysis, the corresponding pooled R2 values were 0.897, 0.942, and 0.992, respectively; this analysis assesses interpolation to an unobserved combination within the tested 3 × 3 composition grid, not extrapolation beyond its factor levels. Recomputed grouped SHAP attribution identified cycle count as the leading input for apparent RDEM (44.94% of relative mean absolute attribution), while the exposure-regime input dominated strength retention (53.36%) and peak-stress retention (56.65%); cycle count × regime was the strongest pairwise interaction in both mechanical targets. At limit states of 60% RDEM and 75% compressive-strength retention, the predicted durability thresholds ranged from 17 to more than 150 cycles, with RDEM governing most cases. The proposed framework pairs crystalline-phase and pore-structure observations with interpretable durability prediction within the tested cyclic sulfate environments. These are exploratory laboratory-cycle thresholds. A 300-resample trajectory bootstrap quantified model-refit variation; neither the thresholds nor their intervals are calibrated to field service time.

GelsVol. 12(11)
Xi'an University of Architecture and Technology (CN)
National Natural Science Foundation of China
Responsible consumption and production
Openalex Percentile: Top 19%
Concrete and Cement Materials Research
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