3.4.2. Dry and Wet Cycle
(1) Appearance
Figure 13 illustrates the progression of surface spalling in SOFS specimens with five different mix proportions over 25 wet–dry cycles. As shown in
Figure 13a–e, the extent of surface deterioration becomes increasingly severe with more cycles, accompanied by more pronounced edge and corner rounding, regardless of the mix proportion. These observations suggest that alternating wet–dry conditions and thermal effects progressively degrade the internal structure of the specimens, resulting in mass loss and strength reduction. Furthermore, the deterioration patterns vary depending on the mix proportion. As shown in
Figure 13a, the H10 specimen exhibited noticeable surface spalling and roughness by the 15th wet–dry cycle. In contrast, the H14 specimen (
Figure 13b) showed only slight edge blunting after 25 cycles, with minimal surface degradation and a relatively smooth surface maintained throughout the test.
Figure 13c suggests that after 10 wet–dry cycles, the H15 specimen developed significant spalling and edge damage, accompanied by interconnection and enlargement of the internal foam cavities. After 25 cycles, deep spalling and distinct grooves were observed.
As shown in
Figure 13d, the SOFS specimen prepared with H18 initially had an uneven surface with visible through-holes. After 10 wet–dry cycles, these holes enlarged and the surface roughness increased; after 25 cycles, evenly distributed large-diameter pores and fine grooves were observed. However, its overall deterioration was less severe than that of H15.
Figure 13e shows similar observations for another H18-prepared specimen, which initially had surface unevenness and through-holes. The progression of damage followed the same trend: pore enlargement and increased roughness after 10 cycles, and uniform distribution of large pores and grooves after 25 cycles, with the damage remaining less severe than that of H15.
Material performance is governed by five key factors: oil sludge residue content, water-to-solid ratio, foaming agent dilution, foam-to-slurry ratio, and mixing time. A higher water-to-solid ratio enhances flowability and surface finish, while a lower foaming agent dilution improves foam stability. An increased foam-to-slurry ratio reduces density, thereby inhibiting moisture migration and heat transfer. An optimized mixing time ensures proper hydration and uniform foam distribution. Among the mixtures, H10 exhibits excellent durability possibly due to its low residue content, optimal water-to-solid ratio, and homogeneous mixing. H14 and H22 maintain structural integrity through sufficient moisture content and enhanced fluidity; notably, the high foam dilution in H22 may contribute to improved density via controlled foam collapse. In contrast, H15 and H18 show compromised performance possibly due to their high residue content, insufficient moisture, and foam instability, leading to macrovoid formation and reduced resistance to cyclic exposure. Based on the observed damage characteristics in
Figure 13, the H14 specimen exhibits the highest resistance to wet–dry cycling among all the evaluated mixes.
(2) Mass Variation Analysis
The structural stability of the specimens under wet–dry cycling varied with the mix proportion, as reflected in the mass loss after 25 cycles: H15 (5.5%), H18 (3.1%), H14 (3.0%), H10 (2.9%), and H22 (2.5%). H22 exhibited the lowest mass loss (2.5%). One-way ANOVA confirmed significant differences among mixtures (F(4,10) = 11.2, p < 0.001), and Tukey HSD test showed H22 lost significantly less mass than H15 (5.5%) and H18 (3.1%) (p < 0.05), while no significant difference was found among H22, H10 (2.9%), and H14 (3.0%).
Critically, H10, H14, and H22 showed better performance possibly due to adequate moisture, thorough hydration, uniform foam distribution, and favorable slurry fluidity, which promoted a homogeneous pore structure. However, the error bars in
Figure 14 reveal greater variability for H10 and H14, suggesting less consistent pore formation and hydration control compared to H22, which displayed a tighter data distribution. This implies that while the average performance of H10 and H14 is acceptable, their reproducibility may be an issue.
In contrast, H15 and H18 suffered from insufficient cement and water, high additive contents, and non-uniform foam generation resulting from a 50× dilution ratio, leading to higher mass loss and wider data scatter. These deficiencies are also evident in
Figure 15, where H22 maintained the highest compressive strength with minimal variability, while H15 and H18 showed poor strength retention.
Figure 16 further confirms the microstructural densification in H22 compared to the fissures observed in H15 and H18.
For an optimized mix design, the error bar analysis underscores that consistency is as critical as mean performance. H22 emerges as the most robust formulation. H10 and H14 require tighter process control to reduce variability, while H15 and H18 are unsuitable for cyclic exposure. Optimization efforts should prioritize a balanced binder content, an optimal foaming agent dilution ratio, and a workable water content to ensure a uniform pore structure and reproducible durability.
(3) Splitting tensile strength analysis
Figure 15 illustrates the progressive decrease in splitting tensile strength and the corresponding strength coefficient with increasing wet–dry cycles for all mixtures, although the degradation rates varied substantially among the five mixes. After 25 cycles, H14 retained the highest residual strength (2.72 MPa), followed by H22 (2.38 MPa), H10 (2.26 MPa), H18 (1.98 MPa), and H15 (1.23 MPa). The strength loss followed the order H22 (12%) < H10 (17%) < H14 (18%) < H18 (26%) < H15 (45%).
One-way ANOVA confirmed significant differences among mixtures in residual splitting tensile strength after 25 cycles (F(4,10) = 26.4, p < 0.001). Tukey HSD post-hoc test showed that H14 (2.72 ± 0.06 MPa) retained significantly higher strength than all other mixtures (p < 0.05). H22 and H10 did not differ significantly from each other (p > 0.05), while both were significantly higher than H18 and H15 (p < 0.05). H15 exhibited the lowest residual strength (1.23 ± 0.21 MPa), significantly worse than all other groups (p < 0.05). The variability patterns reflected in the standard deviations were consistent with the mix designs. H14 and H22 exhibited the lowest variability (SD = 0.04–0.10 MPa), indicating excellent reproducibility and microstructural uniformity. In contrast, H15 displayed the widest variation (SD = 0.15–0.21 MPa), reflecting heterogeneous degradation and unstable pore development—a finding consistent with its insufficient water content (0.29:1) and high residue proportion. H18 showed intermediate variability (SD = 0.10–0.15 MPa).
Statistical analysis is consistent with H14 achieved significantly higher residual strength than H22 (p < 0.05) while maintaining comparably low variability. The superior performance of H10, H14, and H22 may stem from their adequate moisture content, which facilitates complete hydration and produces fine, uniform pore structures that restrict moisture migration. Conversely, H15 and H18 exhibited insufficient hydration products and higher additive proportions, promoting the formation of large, interconnected pores that accelerated moisture transport and thermal stress damage. H14 thus emerges as the optimal formulation, possibly because it simultaneously maximizes residual strength and minimizes performance dispersion, ensuring reliable long-term durability under cyclic environmental loading.
(4) Dry–wet strength coefficient analysis
As shown in
Figure 16, to better illustrate how the strength of the five mixtures evolved over 25 wet–dry cycles, the data were further analyzed and are summarized in
Figure 16 At the 25th cycle, the wet–dry strength coefficients for H10, H14, H15, H18, and H22 were 0.83, 0.82, 0.62, 0.74, and 0.88, respectively. A higher coefficient indicates less strength loss in the cycled specimens relative to the control, while a lower value likely reflects more pronounced degradation.
Comparatively, H22 exhibited the highest coefficient (0.88 ± 0.01), which was significantly higher than all other mixtures (one-way ANOVA, F(4,10) = 18.5, p < 0.001; Tukey HSD, p < 0.05), confirming its superior resistance to cyclic exposure—a finding consistent with its dense microstructure and uniform pore distribution, as discussed earlier. H10 (0.83 ± 0.02) and H14 (0.82 ± 0.02) did not differ significantly from each other, suggesting comparable durability but a slightly greater susceptibility to cyclic effects, likely due to their relatively higher porosity and greater variability in pore structure. H18 showed moderate performance (0.74 ± 0.04), while H15 recorded the lowest coefficient (0.62 ± 0.06), significantly worse than all other groups (p < 0.05), underscoring its poor structural integrity under repeated wetting and drying.
H22 showed the smallest variability (SD = 0.01), confirming its high reliability. H15 exhibited both the lowest mean and largest variability (SD = 0.06), rendering it unsuitable for cyclic environments. Future mix optimization should prioritize reducing variability alongside improving mean strength retention. The ranking of H22 > H10 > H14 > H18 > H15 reinforces the idea that mix designs with a balanced binder content, an appropriate foaming agent dilution ratio, and adequate workability lead to better strength retention. For practical mix optimization, H22 serves as a benchmark. H10 and H14 are acceptable alternatives but would benefit from tighter control over mixing uniformity and porosity. In contrast, H15 and H18 are unsuitable for environments subject to cyclic moisture exposure, possibly due to their substantial strength loss. Future design efforts should focus on the synergistic regulation of the binder dosage, foaming agent ratio, and water content to achieve both high strength retention and low performance variability.
3.4.3. Freeze–Thaw Cycles
Figure 17 illustrates the morphological changes under freeze–thaw cycles,
Figure 18 presents the mass loss variations, and
Figure 19 shows the changes in compressive strength (tested after the completion of the designated freeze–thaw cycles and subsequent conditioning). Through a systematic evaluation of the macroscopic evolution, mass loss rates, and compressive strength degradation, the freeze–thaw resistance of the different SOFS specimens was comprehensively characterized. Statistical analysis (one-way ANOVA followed by Tukey’s HSD post-hoc test) revealed significant differences among the five mixtures in both mass loss (F(4,10) = 18.32,
p < 0.001) and compressive strength retention (F(4,10) = 22.56,
p < 0.001) after 25 freeze–thaw cycles.
H10 exhibited visible spalling after 20 cycles, and by the 25th cycle, interconnected pores had led to gully formation and extensive spalling, with a mass loss of 4.4% ± 1.2%. Its strength retention after 25 cycles was 72.3% ± 1.8%. H14 developed minor spalling after 15 cycles and shallow gullies by the 25th cycle, without any corner or edge damage, accompanied by a mass loss of 4.5% ± 0.3%. Its strength retention was 75.1% ± 2.1%. H15, initially loose with through-pores, began spalling after five cycles and formed deep gullies, corresponding to the highest mass loss of 8.7% ± 0.5% (p < 0.05 compared to all other groups) and the lowest strength retention of 52.4% ± 2.5% (p < 0.05 compared to all other groups). This inferior performance may be attributed to an inadequate water content during mixing, poor workability, and foam coalescence. H18 showed block spalling after 20 cycles and large-area surface spalling with subsurface pore connectivity by the 25th cycle, with a mass loss of 4.6% ± 0.3%. Its strength retention was 65.7% ± 2.2% (p < 0.05 compared to all other groups). H22 initially had corner defects, but after 25 cycles it exhibited only surface spalling without major structural failure, achieving a mass loss of 4.2% ± 0.2% (p < 0.05 compared to all other groups) and demonstrating the highest strength retention of 78.5% ± 1.9%. H10 and H14 did not differ significantly from each other in either mass loss or strength retention (p > 0.05). This performance may be attributed to its dense structure and low porosity, which minimized water ingress and frost heave damage.
The ranking of freeze–thaw resistance differs depending on whether mass loss or strength loss is used as the primary evaluation criterion. Based on mass loss rates (
Figure 18), the order from highest to lowest loss is H15 > H18 > H14 > H10 > H22, whereas based on strength retention (
Figure 19), the order is H22 > H10 > H14 > H18 > H15. This discrepancy arises possibly because mass loss primarily likely reflects surface deterioration and material shedding, while strength loss indicates internal structural integrity and load-bearing capacity. For engineering applications where structural safety is paramount, strength loss is considered the primary criterion for evaluating freeze–thaw resistance, as it directly governs the serviceability and longevity of the material. Accordingly, considering strength retention, mass loss, admixture utilization, and specimen density, the overall freeze–thaw resistance ranking is H14 > H22 > H10 > H18 > H15.