1. Introduction
Self-compacting concrete (SCC) is a highly flowable, non-segregating concrete that fills the formwork and encapsulates the reinforcement under its own weight without mechanical consolidation. SCC is therefore suitable for pre-cast tunnel segments and structural lining applications [
1]. With river sand becoming increasingly scarce, manufactured sand (MS) is widely used as fine aggregate in SCC. Its angular particles and the stone powder finer than 75 μm generated during crushing affect the packing state and deformation behavior of the matrix. For pre-cast segments, the uniaxial post-peak compressive response is a critical indicator, as it reflects the deformation capacity and damage resistance of the material under compression [
2].
Granite powder (GP) in this study refers to the <75 μm stone-powder fraction separated during the production of granite manufactured sand and derived from the same crushed granite as the fine aggregate. This fraction is commonly controlled or removed to meet the fines-content requirement of manufactured sand, and its reuse in cementitious systems has attracted increasing attention, where, depending on the mixture design, such granite-derived powder has been investigated as a supplementary fine material, cement replacement, or sand replacement. At a suitable replacement ratio, GP can fill inter-particle voids, improve packing density, and reduce matrix porosity [
3,
4,
5]. The resulting strength changes reflect the combined effect of filler action, packing modification, and cement dilution [
5,
6]. GP can partially replace fine aggregate without obvious strength reduction and can improve durability when blended with fly ash [
7,
8]. However, the combined performance of GP, expansive agent, and hybrid steel/polypropylene fibers (SF/PPFs) in SCC has not been systematically investigated, and it remains unclear whether the packing benefits of GP are retained in such a coupled fiber-reinforced self-compacting concrete (FR-SCC) system.
Incorporating an expansive agent (EA) is another common approach to reduce the shrinkage of SCC. EA forms expansive hydration products, primarily ettringite, portlandite, and brucite, which under restrained conditions produce a controlled volume expansion that compensates for shrinkage and induces internal self-stress in the hardened matrix. Previous studies on EA-modified SCC and fiber-reinforced SCC indicate that a suitable EA dosage can mitigate shrinkage while maintaining or improving the hardened-state mechanical performance, with the optimum dosage depending on EA chemistry, restraint condition, fiber volume fraction, and matrix composition [
9,
10,
11]. When EA is combined with fibers, the fibers restrain part of the expansive deformation; this restrained expansion has been reported to introduce an internal confinement, or self-stress, in the hardened matrix that may enhance fiber–matrix load transfer and densify the interfacial transition zone in both single-fiber [
12,
13] and hybrid-fiber [
14,
15] systems. However, the dosage-dependent effect of EA on the uniaxial compressive response of FR-SCC has not been conclusively established, particularly when GP is also incorporated into the binder phase.
Hybrid fiber systems combining SF and PPF have been widely used to enhance the post-peak compressive response of SCC. SFs bridge macrocracks and improve ductility, energy absorption, and residual strength, whereas PPFs inhibit microcrack propagation and contribute to energy dissipation [
16,
17]. The uniaxial compressive stress–strain response of SCC reinforced with hybrid SF/PPF or steel–polyvinyl alcohol fibers is sensitive to fiber type, volume fraction, and combination [
17,
18,
19,
20]. For constitutive modeling, the Carreira–Chu equation [
21], the GB 50010 piecewise formula [
22], and Weibull-type damage formulations [
23] have been used to describe full compressive stress–strain curves. Residual-strength correction and elastoplastic-damage extensions have also been proposed for hybrid-fiber concrete [
24,
25].
Although considerable progress has been made, three problems remain unresolved for SCC containing GP, EA, and hybrid SF/PPF. First, the combined effects of GP replacement ratio and EA dosage on the full uniaxial compressive stress–strain response of FR-SCC, especially the post-peak branch, remain insufficiently characterized. Second, limited attention has been paid to the dosage-dependent effect of EA on the compressive ductility of FR-SCC, particularly in GP-containing binder systems. Third, existing studies [
17,
24] generally evaluate the post-peak softening behavior of hybrid SF/PPF-reinforced SCC using total fiber volume fraction, hybrid ratio, or fiber factor, rather than quantifying the individual contributions of
VSF and
VPP through regression. In addition, the consistency between constitutive descending-branch parameters and AE-based damage descriptors has rarely been examined for this material system.
To address these problems, the uniaxial compressive behavior and constitutive modeling of FR-SCC with GP and EA were experimentally investigated. Sixteen mixtures, including 15 FR-SCC mixtures and one fiber-free reference, were prepared as 100 mm × 100 mm × 300 mm prismatic specimens. The experimental design covered systematic variations in GP replacement ratio, EA dosage, and hybrid SF/PPF volume fractions. Uniaxial compression tests with acoustic emission (AE) monitoring were then performed. The objectives were threefold: (i) to characterize the full compressive stress–strain response and quantify the effects of GP, EA, and hybrid SF/PPF on the peak and post-peak parameters; (ii) to compare the fitting accuracy of the Carreira–Chu, GB 50010, and modified Weibull models, to establish two-variable regressions separating the SF and PPF contributions to the ascending- and descending-branch shape parameters, and to develop a ductility-calibrated expression for the descending-branch parameter ad; and (iii) to fit the AE-based damage variable DAE with a two-parameter Weibull cumulative function and to examine the consistency among ad, the AE scale parameter λAE, and the post-peak strain measure ε0.20.
3. Results
3.1. Failure Modes and Stress–Strain Response
The fiber-free reference M12 failed by brittle vertical splitting, with a single dominant longitudinal crack parallel to the loading direction propagating through the matrix–aggregate skeleton (
Figure 4a). Its stress–strain curve (
Figure 5d) shows a nearly linear ascending branch followed by a sharp post-peak drop, and only a short descending segment was captured. M12 also has the lowest peak strain among the 16 mixtures (1.84 × 10
−3,
Table 9).
At the same
VSF and
VPP levels, M1 (without GP and EA) and M9 (12% GP and 8% EA) developed multiple inclined surface cracks with slight corner spalling and no structural disintegration (
Figure 4b,c). M1 reached a higher peak stress, whereas M9 showed a higher peak strain, a lower secant modulus, and a milder post-peak descent (
Table 9). Because the two mixtures had the same
VSF and
VPP levels, these differences are consistent with the influence of GP–EA binder modification on strain capacity and post-peak softening.
The highest-fiber mixture M16 formed a dense network of fine vertical, inclined, and secondary cracks and retained its integrity after loading (
Figure 4d). Its stress–strain curve shows the highest peak strain and a gentler descending branch than M12, M1, and M9, with a wider post-peak strain range. This response is consistent with multiscale crack bridging: PPF can restrain microcrack propagation, whereas SF can bridge macrocracks [
17,
18,
38]. The detailed mechanism is discussed in
Section 4.2.
Figure 5 groups the 16 stress–strain curves by mixture variable. Without GP, increasing the EA dosage from 0% (M1) to 8% (M7) monotonically reduced the peak stress, with little change in the peak strain (
Figure 5a). At an EA dosage of 4%, increasing GP from 0% (M2) to 18% (M6) also reduced the peak stress monotonically (
Figure 5b). At an EA dosage of 8%, the peak stress no longer decreased monotonically and reached a maximum at a 12% GP replacement ratio (M9) (
Figure 5c,
Table 9). With this composition, all fiber-reinforced mixtures (M9 and M13–M16) showed longer descending branches and higher peak strains than the fiber-free reference M12 (
Figure 5d). The post-peak softening varied mainly with
VSF, with the descending branch becoming gentler as
VSF increased from 0.25% to 0.75%, whereas increasing
VPP from 0.05% to 0.15% produced a smaller change in the descending branch. Compared with the changes in peak strain and post-peak softening, the elastic-stage stiffness varied less.
3.2. Effects of Mixture Variables on Compressive Characteristic Parameters
Without GP incorporation, increasing EA from 0% to 8% reduced
fc by 23.9% (from 47.62 MPa for M1 to 36.25 MPa for M7) and decreased
Ec from 30.38 to 26.37 GPa, while
εp remained within 2.26–2.44 × 10
−3. The decrease in
Esec from 19.92 to 16.04 GPa within this EA range was mainly induced by the reduced
fc; and the variations in post-peak performance were directly reflected by the curve profiles in
Figure 5a.
At a constant EA dosage of 4%, increasing the GP replacement ratio from 0% (M2) to 18% (M6) monotonically reduced
fc by 17.9% (from 42.07 MPa to 34.52 MPa) and decreased
Ec from 28.82 to 26.05 GPa, whereas
εp remained within 2.14–2.44 × 10
−3. In contrast, at a fixed 8% EA dosage,
fc no longer declined monotonically and reached its maximum at 12% GP (M9: 39.52 MPa). Similarly,
εp peaked at the same GP replacement ratio (M9: 2.58 × 10
−3), which was higher than the values of 2.17–2.28 × 10
−3 obtained at the other four GP replacement ratios. These results indicate that the GP–EA combination in M9 gave the most favorable binder composition for the uniaxial compression tests in this study. The intrinsic interaction mechanism between GP and EA in modifying matrix performance is discussed in
Section 4.
With the favorable binder composition (12% GP and 8% EA), the hybrid SF/PPF system exerted a more prominent effect on peak strain and post-peak softening than on peak stress. Compared with the fiber-free M12, the M16 mixture with the highest fiber volume fractions increased εp by 76.6% (from 1.84 × 10−3 to 3.25 × 10−3) and reduced Esec by 41.3% (from 19.58 GPa to 11.49 GPa), while fc slightly fluctuated within 35.97–39.76 MPa. Within the tested range, increasing VSF produced a greater increase in εp than increasing VPP. At a fixed VPP, increasing VSF from 0.25% to 0.75% increased εp by 61.2% (M13 to M15) and 40.1% (M14 to M16). In contrast, increasing VPP from 0.05% to 0.15% at a fixed VSF only increased εp by 18.4% (M13 to M14) and 2.8% (M15 to M16).
Across the five Series II mixtures, the
εp and
Esec were expressed as linear functions of
RIv, as given in Equations (2) and (3).
The moderate
R2 values indicate that one aspect-ratio-weighted descriptor does not separate the differing effect magnitudes of
VSF and
VPP; this limitation is revisited in
Section 3.5.2.
Across the 16 mixtures,
Ec ranged from 25.05 to 30.38 GPa (average 27.2 GPa). The mixture variables had a smaller effect on the elastic-regime stiffness than on the peak and post-peak parameters. The quantitative ductility and energy-dissipation indices are analyzed in
Section 3.3.
3.3. Post-Peak Ductility and Energy Dissipation
The post-peak energy and ductility of the 16 mixtures were quantified using the parameters summarized in
Table 10.
The energy and ductility parameters are defined as follows. The pre-peak and post-peak energy densities
Wpre and
Wpost are the areas under the stress–strain curve from the origin to
εp and from
εp to a fixed ultimate strain
εu, with
Wtotal =
Wpre +
Wpost. The post-peak ductility ratio
μ85 is defined by Equation (5), where
ε0.85 is the strain at which the stress descends to 0.85
fc on the post-peak branch. Following Cui et al. [
24], the residual strain
ε0.20 is the strain at which the stress descends to 0.20
fc. Following the energy-ratio toughness-index approach for fiber-reinforced concrete [
39], the toughness index
TI is defined as the ratio of total to pre-peak energy density. The numerical integration was performed using the trapezoidal rule on the raw stress–strain data with a (0, 0) origin, taking
εu = 0.015 for curves that reached this strain; for curves terminating earlier, the integration was carried out up to the measured terminal strain without extrapolation.
From the fiber-free reference M12 to the highest-fiber mixture M16 with the same binder composition,
Wpost rose from 0.029 to 0.222 MPa, by a factor of 7.66;
ε0.20 increased from 2.93 × 10
−3 to 14.40 × 10
−3, by a factor of 4.92; and
TI increased from 1.75 to 3.48. Meanwhile,
Wpre increased by a factor of 2.37,
ε0.20/
εp from 1.59 to 4.43, and
μ85 from 1.14 to 1.48 (
Table 10). The larger increase in
Wpost than in
Wpre indicates that hybrid SF/PPFs mainly improved the post-peak response rather than the pre-peak regime.
Within the M12–M16 series with the favorable binder composition, the absolute energy and strain measures (Wpost, Wtotal, ε0.20, and μ85) reached their maxima at M16, whereas TI peaked at M15 (3.58) and decreased slightly at M16 (3.48). This decrease occurs because the larger εp of M16 raised Wpre and thus lowered the post-peak weighting in TI, although its absolute Wpost was the largest. TI therefore reflects the relative post-peak contribution rather than its absolute value.
Within Series I, the 11 mixtures M1–M11 had the same fiber volume fractions (VSF = 0.50% and VPP = 0.10%; RIv = 71.2) but differed in GP replacement ratio and EA dosage. The coefficients of variation of μ85 and TI across these mixtures were only 3.5% and 5.3%, respectively, indicating limited variation in the pre-/post-peak energy partitioning under fixed fiber volume fractions. In contrast, the absolute energy parameters Wpre, Wpost, and Wtotal showed coefficients of variation of 16–19% and correlated with fc (r = 0.932 between fc and Wtotal). The influence of binder composition was therefore mainly reflected in the magnitude of energy absorption through its association with fc, whereas the pre-/post-peak partitioning varied less under the fixed hybrid-fiber system.
The dependence of
TI and
ε0.20/
εp on
RIv is presented in
Figure 6. Linear regressions on the 16 mixtures give Equations (8) and (9), with
RIv entered as percentage values via Equation (1).
The positive slopes indicate that higher RIv was associated with higher TI and higher ε0.20/εp. The moderate R2 values reflect the clustered RIv design and the fact that RIv does not distinguish the mechanical roles of SF and PPF; for example, M14 has a relatively high RIv (74.3) owing to the high PPF aspect ratio, yet its ε0.20/εp (2.68) is lower than those of M15 and M16. Therefore, RIv should be treated only as a first-order descriptor.
These macroscopic ductility and energy indices provide the basis for the subsequent AE damage analysis.
3.4. Acoustic Emission Characteristics and Damage Evolution
The AE signals recorded during loading were used to characterize the evolution of internal cracking. AE monitoring has been widely used to track damage development in fiber-reinforced concrete under axial loading [
40,
41]. The AE response is first divided into loading stages and then used to define an AE-based damage variable, which is fitted with a two-parameter Weibull distribution.
3.4.1. Stage-Wise Division of the Acoustic Emission Response
In
Figure 7, the dashed lines mark the times at which the axial stress first reaches 0.30
fc and 0.80
fc, used here as operational thresholds rather than universal damage limits. They define three stages: Stage I (0–0.30
fc), a low-activity stage associated with seating, defect closure, and possible early microcracking; Stage II (0.30–0.80
fc), stable microcrack propagation; and Stage III (0.80
fc through the descending branch), accelerated crack coalescence, peak formation, and post-peak softening. This division follows the AE framework of RILEM TC 212-ACD [
37] and earlier AE studies of concrete under compression [
42].
Stage I accounted for about 1% or less of Σ
CAE in all four specimens, indicating that low-stress microcracking contributed little to the total recorded activity. Stage II contributed 3.0–15.1%, and Stage III accounted for 83.9–96.5% (
Figure 7). The Stage III dominance suggests that the recorded AE activity was concentrated near the peak and during post-peak softening rather than at low stress.
The peak per-second ring count
CAE increased from 110 for the fiber-free M12 to 1059 for M16, about ten times higher. The total ring count
Nu for M12 (4072) was far below those of the fiber-reinforced mixtures (63,000–181,000), consistent with its shorter post-peak history and brittle, localized failure. Therefore, the absolute AE count of M12 should be interpreted separately from those of the fiber-reinforced mixtures, for the reasons discussed in
Section 3.4.2.
3.4.2. AE Damage Variable and Weibull Evolution
An empirical AE-based damage variable is defined as the normalized cumulative ring count:
where
N(ε) is the cumulative ring count at axial strain
ε and
Nu is the cumulative ring count at the end of loading. The ring-count record (1 s sampling) and the stress–strain record were mapped onto a common strain axis by linear interpolation, with the ascending and descending branches treated separately.
Following the statistical damage treatment used for concrete under compression [
24], the AE damage evolution was fitted with a two-parameter Weibull cumulative distribution:
where
mAE is the shape parameter, controlling the concentration of damage accumulation in strain, and
λAE is the scale parameter, the characteristic strain at which the fitted
DAE reaches 1 − e
−1 ≈ 0.632 rather than a failure strain. Equation (11) was fitted to the 16 normalized AE–strain curves by non-linear least squares; the fitted
mAE,
λAE, and
R2AE are listed in
Table 11, and
Figure 8 shows the measured and fitted
DAE–
ε curves for the four representative specimens.
All 16 fits gave R2AE above 0.94 (mean 0.969). For the 15 fiber-reinforced mixtures, mAE fell within a narrow range of 1.135–1.509, indicating that the AE damage accumulated progressively over a broad strain range, consistent with their distributed cracking. The fiber-free M12 had mAE = 5.628, about 3.7 times the largest fiber-reinforced value, consistent with its more concentrated damage accumulation and brittle failure.
The scale parameter λAE ranged from 1.748 × 10−3 (M12) to 11.531 × 10−3 (M16), spanning nearly a factor of seven, and varied consistently with the post-peak deformation capacity of the mixtures. M12 gave the lowest value, whereas the high-VSF mixtures M15 and M16 gave the two highest values. Within Series I, M9 gave the highest λAE (7.187 × 10−3), consistent with its higher εp and flatter post-peak slope noted above. This suggests a contribution of the favorable GP–EA binder composition to deformation capacity at the same VSF and VPP levels.
Across the 16 mixtures,
λAE was linearly associated with the macroscopic residual strain
ε0.20 (
r = 0.987). The corresponding correlation restricted to the 15 FR-SCC mixtures is examined in the cross-method consistency check in
Section 3.5.3. This association indicates that
DAE(ε) can serve as an empirical AE-based counterpart to the macroscopic post-peak descriptors used in the constitutive analysis. For each mixture, three replicate specimens were tested, and the AE results reported here (
Figure 7 and
Figure 8,
Table 11) were taken from the same representative specimen (the median-peak-stress replicate) defined in
Section 2.5. Because the absolute AE counts depend on the recorded post-peak duration, the degree of crack localization, and signal attenuation along the propagation path, the cumulative and per-second ring counts are expected to show larger specimen-to-specimen scatter than the normalized damage variable. Expressing the AE response through the normalized damage variable
DAE reduces the sensitivity to the absolute count level and yields the more reproducible shape descriptors
mAE and
λAE, which is why the subsequent analysis is based on
DAE rather than on absolute counts. Given the limited number of replicates (three per mixture), the AE parameters and the AE-based correlations in
Section 3.5.3 are regarded as consistency trends within the present dataset rather than as population estimates.
3.5. Constitutive Modeling
The post-peak stress–strain response analyzed above is next described using parametric constitutive models, and the AE-based descriptor is then used for a cross-method consistency check with the constitutive and macroscopic post-peak parameters. This section proceeds in three steps: parameter calibration on the 16 representative curves, regression of the model parameters against fiber volume fractions and post-peak ductility, and a cross-method consistency check among the constitutive, AE-based, and macroscopic post-peak descriptors.
3.5.1. Comparison of Three Constitutive Models
Three constitutive forms with different theoretical bases were fitted to the 16 normalized stress–strain curves: the single-shape-parameter Carreira–Chu rational model [
21], the piecewise GB 50010 model [
22], and a modified Weibull damage model with residual correction [
24]. Comparable frameworks for hybrid-fiber UHPC [
43] and hybrid-fiber cementitious composites [
44] provide related constitutive-modeling references. Each model was fitted independently for every mixture by non-linear least squares on
ξ =
ε/
εp and
η =
σ/
fc, using the three-replicate mean
fc and
εp from
Table 9 for normalization.
The Carreira–Chu form is
where
β is the shape parameter controlling both the ascending and descending branches. The GB 50010 form is piecewise:
with two parameters
aa and
ad controlling the ascending and descending branches separately. The modified Weibull form, in its normalized version, is
where
a is the damage correction coefficient,
mσ is the Weibull shape parameter, and
vw =
u0/
εp is the normalized Weibull characteristic strain. The normalizing constant
c enforces
η(1) = 1.
The fitted parameters and coefficients of determination are listed in
Table 12. On the 15 FR-SCC mixtures, all three forms gave high fitting precision, with mean
R2 of 0.976, 0.995, and 0.980 for the Carreira–Chu, GB 50010, and modified Weibull forms, respectively. The fiber-free reference M12 was fitted with
R2 of 0.938, 1.000, and 0.982, but its
β = 9.96 and
ad = 18.08 fall well outside the FR-SCC parameter window (
β = 2.5–4.1,
ad = 1.09–3.50), reflecting its brittle response (
Table 12, footnote
1). The post-peak range of M1 terminated earlier at
ε = 9.55 × 10
−3 (footnote
2), which affects its modified Weibull residual coefficient.
GB 50010 was adopted as the primary FR-SCC constitutive model for three reasons: its mean
R2 = 0.995 (minimum 0.985 among the 15 FR-SCC mixtures) was the highest of the three forms; its piecewise parameters
aa and
ad describe the ascending and descending branches separately, making them suitable regression targets in the next subsection; and it is widely used in Chinese engineering practice. The Carreira–Chu and modified Weibull fits are retained as reference benchmarks in
Table 12. The measured stress–strain curves and the three constitutive fits for four representative FR-SCC specimens are compared in
Figure 9. The modified Weibull form was not adopted as the primary model: beyond its lower mean
R2, the residual-stiffness term
cξ(1 −
a) in Equation (14) becomes dominant at strains far beyond the measured range, which restricts extrapolation but did not govern the fitted response within the measured strain range.
3.5.2. Fiber-Volume-Fraction-Based and Ductility-Calibrated Regression of GB 50010 Parameters
The two GB 50010 shape parameters aa and ad were used as regression targets to examine the apparent contributions of VSF and VPP within the present mixture design, fitted on the 15 FR-SCC mixtures (M12 excluded as the fiber-free reference). An auxiliary regression of ad on ε0.20/εp is also reported for use when post-peak test data are available.
A two-variable linear regression of
aa on
VSF and
VPP gives:
with
VSF and
VPP in vol.%,
R2 = 0.927 and adjusted
R2 = 0.915. On a per-vol.% basis, the fitted PPF coefficient is about 2.9 times the SF coefficient; however, over the tested ranges (
VSF 0.25–0.75 vol.%,
VPP 0.05–0.15 vol.%), the predicted contribution of SF to
aa is comparable to that of PPF because the SF range is wider. The PPF coefficient is therefore interpreted as a per-unit-volume sensitivity of
aa to fine fibers, qualitatively consistent with the smaller diameter and larger specific surface area of PPF, rather than as evidence that PPF governs
aa. Since the binder variables (GP and EA) are not included in Equation (15), this coefficient reflects an apparent sensitivity rather than a mechanistic SF–PPF separation. A single-variable regression of
aa on
RIv gives
R2 = 0.819, indicating that
RIv retains most of the variance but does not resolve the separate
VSF and
VPP contributions.
A two-variable linear regression of
ad on
VSF and
VPP gives:
with
R2 = 0.778 and adjusted
R2 = 0.741. The
VSF coefficient is the larger in magnitude and is negative, indicating that increasing
VSF flattens the descending branch, consistent with the post-peak crack-bridging contribution of hooked steel fibers. The
VPP coefficient is small, suggesting a limited apparent contribution of PPF to the descending-branch shape over the tested range. When the measured ductility ratio
ε0.20/
εp is available, the alternative regression
reaches a higher
R2 = 0.943 (adjusted
R2 = 0.939), because
ε0.20/
εp directly samples the measured descending branch that Equation (16) only approximates from composition. Equation (16) requires only the fiber volume fractions and is retained as the fiber-volume-fraction-based predictor, whereas Equation (17) is the ductility-calibrated form usable once post-peak test data are obtained.
The in-sample reconstruction accuracy of Equations (15)–(17) was evaluated at the curve level by substituting them into Equation (13) and comparing with each measured trace (
Figure 10). Across the 15 FR-SCC mixtures, the fiber-volume-fraction-based form (Equations (15) and (16)) gave a mean curve-level
R2 of 0.955 (all specimens above 0.84), and the ductility-calibrated form (Equations (15) and (17)) gave a mean of 0.972 (all above 0.912). The minimum occurred at M15 for the fiber-volume-fraction-based form and at M13 for the ductility-calibrated form. The fiber-volume-fraction-based form is suitable for preliminary in-sample curve screening within the tested calibration window, whereas the ductility-calibrated form gives more reliable reconstructed curves.
Because Equations (15)–(17) were calibrated and assessed on the same 15 FR-SCC mixtures, leave-one-out cross-validation (LOOCV) was carried out to check their robustness against overfitting. In each fold the regression was refitted on 14 mixtures and used to predict the parameter of the single mixture left out, and the predictive coefficient of determination (
Q2) and the root-mean-square error (RMSE) were computed from the held-out predictions. For the ascending-branch regression (Equation (15)) the in-sample
R2 of 0.927 decreased only to
Q2 = 0.859 (RMSE from 0.084 to 0.116); for the fiber-volume-fraction-based descending-branch regression (Equation (16))
R2 = 0.778 decreased to
Q2 = 0.733 (RMSE from 0.318 to 0.349); and for the ductility-calibrated regression (Equation (17))
R2 = 0.943 decreased to
Q2 = 0.919 (RMSE from 0.161 to 0.191). The small reductions, with the cross-validated error concentrated in the corner mixtures M13–M16 of the clustered fiber design, indicate that the regressions did not show severe overfitting and support interpolation within the calibrated composition window, the ductility-calibrated Equation (17) being the most robust. This LOOCV is an internal robustness check rather than independent external validation; validation on independent specimens, as noted in
Section 4.4, remains future work.
The validity of Equations (15)–(17) is restricted to the experimental window of this study: VSF 0.25–0.75 vol.%, VPP 0.05–0.15 vol.%, ε0.20/εp 2.46–4.43, and RIv 35.6–106.8. Equation (16) is intended for in-sample composition screening before specimens are prepared and Equation (17) for refined prediction after benchmark mixtures are tested.
3.5.3. Cross-Method Consistency Among Constitutive, Acoustic Emission and Ductility Descriptors
The GB 50010 descending-branch parameter ad, the AE characteristic strain λAE, and the macroscopic residual strain ε0.20 describe related but non-identical aspects of the post-peak response. Two pairwise checks were performed on the same 15 FR-SCC mixtures, with M12 excluded as the fiber-free reference.
The first check pairs
ad with
λAE. A larger
ad corresponds to a steeper descending branch, whereas a larger
λAE indicates a larger characteristic strain scale for cumulative AE damage, so a negative correlation is expected. The linear regression gives
with
λAE in 10
−3, a negative Pearson correlation coefficient of −0.904 (
n = 15, 95%
CI [−0.968, −0.730],
p < 0.001), and
R2 = 0.817. The negative sign is consistent with a steeper descending branch corresponding to a smaller AE characteristic strain scale, and the magnitude indicates a close cross-method relationship between the constitutive descending-branch shape and the AE characteristic strain scale. This relation is therefore interpreted as a cross-method consistency check.
The second check pairs
λAE with the macroscopic residual strain
ε0.20. Both quantities locate damage development on the strain axis, so a positive relation is expected. The linear regression on the 15 FR-SCC mixtures gives
with both
λAE and
ε0.20 in 10
−3,
r = +0.983 (
n = 15, 95%
CI [+0.949, +0.995],
p < 0.001) and
R2 = 0.967, indicating a close linear association between the AE and macroscopic strain scales. This represents a strain-scale consistency check that complements the shape-based check in Equation (18).
The two checks examine different facets of the same post-peak loading history. These checks are not independent validation, because the descriptors share the same loading history; their simultaneous agreement indicates that ad tracks post-peak behavior that is also captured by the AE and ductility measures.
For completeness, the modified Weibull shape parameter
mσ (
Table 12) correlates with
mAE (
Table 11) at
r = +0.471 (
n = 15,
p = 0.076) across the same 15 mixtures, and the characteristic strain
u0 =
vwεp correlates with
λAE at r = +0.497 (
n = 15,
p = 0.059). These weaker correlations are not statistically significant at the 0.05 level and are reported only as supplementary benchmarks, consistent with the choice of GB 50010 as the primary constitutive form. To the authors’ knowledge, this specific constitutive–AE consistency check has rarely been reported for FR-SCC incorporating GP, EA, and hybrid SF/PPF.
3.6. Microstructural Evidence for the Role of GP and EA
To clarify the respective roles of GP and EA, the hardened FR-SCC was characterized by X-ray diffraction (XRD; X’Pert3, PANalytical B.V., Almelo, The Netherlands; Cu Kα, 5–90° 2θ) on bulk powders and by scanning electron microscopy (SEM; MIRA, TESCAN, Brno, Czech Republic) on the fracture surfaces of the post-test prisms, using the GP0, GP12 and GP18 mixtures (M7, M9 and M11, all at 8% EA) as a representative series in which only the GP content varies. No energy-dispersive X-ray spectroscopy was performed, so all phase and fiber assignments below are inferred from morphology and the XRD peak positions and are not confirmed by elemental microanalysis.
Figure 11 compares the XRD patterns; the main reflections were assigned from their characteristic 2θ positions to ettringite (AFt, ~9.1°), portlandite (CH, ~18.0°), quartz (~26.6°) and calcite (~29.4°). The portlandite peak did not decrease with increasing GP content and was strongest for the GP18 mixture; since a pozzolanic reaction would consume portlandite, this absence of any reduction indicates that, under the present materials, age and detection conditions, the GP behaved predominantly as a filler rather than as a pozzolanic addition, consistent with its limited reactivity (28-day activity index of 76.7%). Any residual pozzolanic contribution is therefore more likely dominated by the fly ash than by the GP. At a fixed GP content the ettringite peak increased with EA dosage (from 22.4 to 28.2 at GP0 and from 19.2 to 27.4 at GP12 in semi-quantitative peak-area units), consistent with additional ettringite formation associated with the EA and in line with the restrained-expansion mechanism discussed in
Section 4.1. The quartz reflection originates mainly from the manufactured-sand and GP grains and is not used as a tracer of GP content, whereas the calcite peak is attributed to secondary carbonation during sample exposure and preparation rather than to primary hydration.
The filling action of GP is shown in
Figure 12. In the GP0 mixture only the coarse manufactured-sand grains are present and the matrix appears comparatively loose and porous, whereas with 12% GP the inter-particle voids are densely occupied by fine angular powder grains and the matrix becomes markedly denser and more compact; at 18% GP the matrix is still filled but spherical entrapped-air voids and air-void imprints become more frequent, indicating that the filling benefit is subject to an optimum dosage. In all cases the GP grains show angular, brittle fracture surfaces (locally conchoidal) and clean particle–matrix boundaries; no reaction rim was resolved at the SEM scale examined, consistent with a predominantly physical filling and packing action that refines the pore structure and increases the packing density, while any low-level chemical contribution was below the resolution of the present SEM/XRD observations.
The fiber–matrix and aggregate–matrix interfaces are shown in
Figure 13. The polypropylene fibers (nominal diameter 31 µm) are partly coated with hydration products but exhibit longitudinal fibrillation and debonding near the fiber root, and the steel fibers (nominal diameter ≈ 0.55 mm) present a smooth surface and a clean debonding gap with smooth pull-out channel walls; in neither case was a reaction layer observed at the fiber surface, and the spherical fly-ash particles and the GP and sand grains likewise debonded cleanly. The post-fracture morphology indicates that load transfer at these interfaces was dominated by mechanical interlock and friction, whereas chemical adhesion was not directly evidenced by the present SEM images; the interfacial behavior was also spatially variable, ranging from debonding gaps (indicating a weaker interface) to crack propagation through the matrix (indicating a locally stronger interface).