3.1. Characterization of Waste PVC Additives (SEM, EDS, and XRD Analysis)
The morphological characteristics, elemental composition, and mineralogical structure of the waste PVC foils were investigated using Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Spectroscopy (EDS), and X-Ray Diffraction (XRD). The surface microstructures of the waste additive are presented in
Figure 5.
As seen in
Figure 5, the waste PVC surface exhibits a highly irregular and undulated morphology characterized by directional striations. These surface features are attributed to the mechanical stresses applied during the original thermoplastic extrusion or calendering processes. A significant presence of bright phases and surface protrusions was observed, creating a rough surface texture which is critical for physical interlocking with the binder.
EDS analysis was conducted to identify the chemical nature of these protrusions. The elemental composition data are summarized in
Table 7 and
Figure 6.
As shown in
Table 7, the material contains a substantial mineral filler content, with Calcium (Ca) constituting approximately 26% by weight. The EDS spectrum is dominated by Carbon and Oxygen peaks, implying the polymeric matrix and carbonate structure. To definitively identify the crystalline phase of these calcium-based fillers, XRD analysis was performed. The resulting diffraction pattern is illustrated in
Figure 7.
The XRD analysis exhibits a sharp, high-intensity diffraction peak at 2-θ = 29.52°. This specific angle corresponds to the characteristic (104) plane of Calcite (CaCO
3) [
45]. This mineralogical finding corroborates the high Calcium and Oxygen concentrations observed in the EDS analysis (
Figure 8 and
Figure 9), implying that calcium carbonate is the primary filler material used in the PVC formulation.
The presence of rigid crystalline Calcite fillers within the polymer matrix is expected to enhance the stiffness of the waste additive, potentially contributing to the rutting resistance of the modified mixture. In addition, Calcite-containing mineral fillers are known to improve rutting resistance [
46,
47].
The exposed Calcite particles on the foil surface provide polar active sites. Unlike smooth, purely polymeric surfaces, these mineral sites may contribute to improved physio-mechanical interaction with the asphalt binder; however, no direct adhesion measurements were conducted to quantitatively imply this effect.
The combination of the inherently hydrophobic nature of PVC and the surface roughness induced by filler particles results in a textured surface morphology. Although such characteristics may influence wettability behavior, the potential formation of a “Cassie–Baxter” state and its effect on contact angle were not directly evaluated in this study. Therefore, any associated improvement in moisture resistance should be interpreted as a possible mechanism rather than a directly verified outcome.
3.2. Hamburg Wheel Tracking Test Results and Evaluation
The HWTT was performed in water at 50 °C. The rut progression curves plotted by averaging the deformations (left and right wheel) are given in
Figure 10. Furthermore, common index parameters from HWTT results were calculated and presented in
Table 8.
The HWTT was conducted in accordance with AASHTO T 324 using the wet test method. The termination threshold was set at a maximum rut depth of 20 mm or 20,000 passes. It was observed that both control and modified mixtures reached the 20 mm failure limit at approximately 5000 passes. Considering that the tests were performed submerged in water without the addition of any anti-stripping agents or secondary additives, these results are considered reasonable and representative of severe moisture-induced stress.
It should be noted that AASHTO T 324 does not prescribe a universal pass/fail criterion for the number of loading cycles, as such limits are typically defined by regional specifications. In the Turkish Highway Technical Specifications issued by the General Directorate of Highways (KGM), a rut depth limit of 4.5 mm at 20,000 passes is specified for dry Hamburg Wheel Tracking tests conducted at 60 °C using 50 mm thick specimens. However, a corresponding limit value for the wet test condition has not been explicitly defined. Therefore, in this study, the performance of the mixtures under wet HWTT conditions was evaluated based on their relative resistance to deformation and moisture-induced damage by comparing the stripping behavior and failure points of the modified mixtures with those of the control mixture.
The HWTT results suggest that the geometric configuration of waste PVC additives may influence the thermo-mechanical performance and moisture susceptibility of asphalt mixtures. When analyzing the resistance to permanent deformation through Creep Slope (CS) and total deformation values, the fibrous structure of wiry PVC particles provided a distinct reinforcement mechanism within the asphalt matrix. The mixture containing 12.5% wiry PVC exhibited superior structural stability among all tested samples, achieving the lowest CS value of 0.00137 mm/cycle and limiting total deformation to 9.44 mm, which represents a substantial improvement over the control sample’s CS of 0.002113 mm/cycle and deformation of 14.56 mm. This behavior indicates that the wiry geometry effectively distributes shear stresses and delays the accumulation of rutting through a bridging effect between aggregates.
In contrast to the consistent stability observed in the wiry series, the mixtures modified with random geometry PVC displayed considerable variability and instability in their deformation behaviors. While the 7.5% random addition yielded an optimal resistance with a reduced CS of 0.0018775 mm/cycle, deviations from this specific ratio resulted in marked performance deterioration. Notably, the deformation curves for the 12.5% random mixture reveal a rapid descent into the stripping phase, suggesting that high concentrations of randomly cut plastics with larger surface areas may disrupt the aggregate-binder adhesion rather than reinforcing it. This is further evidenced by the 5% random sample, which performed worse than the control mixture with a total deformation of 16.96 mm, implying the sensitivity of the matrix to the random additive ratio.
The moisture susceptibility of the mixtures was further characterized by the Stripping Inflection Point (SIP) and the Stripping Slope (SS), where a higher SIP indicates prolonged resistance to water damage [
48]. The data reveals that wiry additives generally maintained or improved the stripping resistance compared to the control value of 2515 cycles, with the 5% wiry sample reaching a SIP of 3025 cycles. However, the 12.5% random mixture exhibited a critical premature failure with a SIP of only 1775 cycles, followed by a steep stripping slope that indicates a rapid loss of adhesion under hydrodynamic pressure. Consequently, the comprehensive analysis suggests that wiry geometries are preferable for enhancing the internal cohesion and service life of the pavement, whereas random geometries pose a risk of accelerated moisture-induced damage if not utilized at the precise optimum content.
3.3. Repeated Creep Test Results and Evaluation
A Repeated Load Creep Test was conducted to evaluate the permanent deformation resistance of asphalt mixtures modified with waste PVC coating materials of varying geometries (fibrous and random). The experiments were performed at a test temperature of 40 °C. To ensure the accuracy and reproducibility of the results, three identical asphalt specimens were tested for each additive configuration. The load repetition–deformation curves presented in
Figure 11 were plotted using the arithmetic mean of the data obtained from these three replicate specimens.
Upon examining the Repeated Load Creep Test results presented in
Figure 11, it is evident that the geometry and content of waste PVC significantly influence the permanent deformation behavior.
For both waste geometries (wiry and random), the lowest permanent deformation values were obtained at the 7.5% additive content. At lower dosages (5% and 7.5%), the reinforcement effect of the fibrous (wiry) structure provided a significantly superior performance compared to the random structure. Specifically, at the 7.5% content, wiry samples exhibited approximately 22% lower total deformation than random samples, indicating enhanced shear resistance. Similarly, the wiry geometry offered a 14% performance advantage at the 5% content.
One of the most notable findings of the analysis is the reversal of performance when the additive content exceeds 10% (up to 12.5%). The graphs reveal that mixtures with 10% and 12.5% contents (both wiry and random) exhibited higher deformation values compared to the Control (unmodified) specimen. This suggests that excessive plastic volume within the matrix weakens aggregate interlocking, effectively creating slip planes that accelerate deformation.
The creep slopes calculated from the secondary (linear) region of the deformation curves reflect the stability of the mixtures under long-term loading. Consistent with the total deformation results, the lowest creep slope values were calculated for the 7.5% Wiry (0.000014 mm/cycles) and 5% Wiry (0.000015 mm/cycles) specimens. A lower creep slope values are generally associated with greater resistance to viscoplastic behavior. Conversely, the increase in slopes when deviating from the optimum content implies the mixture’s increased susceptibility to rutting.
3.4. Modified Lottman Test Results and Evaluation
Figure 12 illustrates the effects of different waste PVC foil geometries (random and wiry) and varying additive contents on the Indirect Tensile Strength (ITS) and Tensile Strength Ratio (TSR) of the asphalt mixtures. The obtained data reveal that both fiber geometry and dosage are decisive parameters influencing mechanical performance and moisture resistance.
A comparative analysis of
Figure 12 shows that wiry-shaped waste PVC additives are more effective in enhancing the mixture’s resistance to tensile stresses compared to random-shaped additives. Due to their low aspect ratio and irregular structure, random geometry particles failed to create a sufficient reinforcement effect within the aggregate skeleton; consequently, their ITS values followed a horizontal trend similar to the control sample levels (approximately 1100 kPa). Conversely, wiry fibers, by virtue of their morphology, facilitated stronger mechanical interlocking between the aggregate and the bitumen matrix. This mechanism hinders the pull-out of fibers under loading, allowing tensile stresses to be dissipated over the fibers and thereby increasing overall strength.
For both series, the 7.5% additive rate emerges as a critical threshold regarding performance evolution. Particularly in the wiry fiber series, ITS values exhibited a linear escalation as the content increased from 0% to 7.5%, reaching a peak point at approximately 1500 kPa. This improvement can be attributed to the enhancement of binder cohesion via polymer modification and the crack-arresting effect of the fibers.
However, as the additive content exceeded the optimum value, reaching 10% and 12.5%, a precipitous decline in mechanical performance was observed in both series. Consistent with the existing literature, this phenomenon is primarily caused by the inability of high plastic content to distribute homogeneously within the mixture, leading to agglomeration. These plastic clusters create weak spots that are not fully wetted by bitumen, disrupting the structural continuity of the mixture and reducing its load-bearing capacity.
When examining the TSR results, which characterize the mixture’s durability against moisture, it is observed that the 7.5% wiry PVC addition improved the bitumen–aggregate interfacial adhesion, elevating the TSR value to the 85% level (surpassing the control sample). The use of hydrophobic PVC material at this optimum ratio effectively limited water penetration into the mixture body. However, increasing the dosage further (10–12.5%) reduced the coating ratio of the bitumen film over the aggregates, facilitating water ingress at the interface and causing stripping. This is corroborated by the fact that the TSR values of high-dosage samples dropped below the critical 75% threshold.
In conclusion, the utilization of waste PVC foils with a “wiry” geometry at a limiting dosage of 7.5% has been determined as the optimal engineering solution for maximizing dry strength (ITS) while simultaneously maintaining resistance to water damage (TSR).
3.5. Semi-Circular Bending Test Results and Evaluation
The SCB test was conducted to evaluate the fracture resistance of the asphalt mixtures. Load–displacement curves of the asphalt mixture samples are shown in
Figure 13. The peak load values and standard deviations obtained from these tests are presented in
Figure 14. The results indicate that it is evident that the incorporation of waste PVC is associated with an improvement in the load-bearing performance of the samples compared to the control mixture. From a geometric perspective, the “Wiry” type additive appears to provide more effective interlocking mechanism within the matrix compared to the “Random” type, resulting in higher strength values. The data indicate that the optimum waste PVC content is approximately 7.5%. Beyond this ratio—specifically, at 10% and 12.5% contents—a loss in strength was observed. This decrease may be related to the weakening of binder–aggregate adhesion and/or the tendency of PVC particles to agglomerate at elevated dosages.
Using the load–displacement curves obtained from the SCB tests, the fracture energy (Gf) was calculated, serving as a critical parameter to define the asphalt concrete’s resistance (toughness) against crack propagation. As illustrated in
Figure 15, the use of waste PVC increased the fracture energy in all modified mixtures compared to the control sample, which had a value of 1355 J/m
2. This improvement suggests that waste PVC particles enhance the energy absorption capacity by impeding crack propagation or extending the crack path within the matrix. The impact of particle geometry was significant; the performance of “Wiry” (fibrous) waste was markedly superior to that of “Random” particles. For instance, at a 7.5% addition rate, while the “Random” series provided a 50% increase over the control (2033 J/m
2), the “Wiry” series at the same rate achieved a 144% increase, reaching the highest observed value of 3301 J/m
2. This disparity is explained by the effective bridging mechanism formed by the fibrous PVC structure across crack surfaces, which significantly enhances the ductility of the specimen.
To further characterize the cracking potential, the slope at the inflection point (|m|) and the Flexibility Index (FI) were analyzed.
Figure 16 presents the variations in slope values. The results indicate that waste additives affect the cracking resistance of asphalt mixtures, depending on the geometry and content rate. The reference control sample exhibited a brittle behavior with an FI value of 6.47. In the literature, FI values below 10 are generally regarded as indicators of high brittleness and weak resistance to crack propagation [
37,
40]. Conversely, both additive types improved the mixture’s energy damping capacity. The performance of the “Wiry” additive was particularly notable; at 7.5% content, it not only maximized fracture energy but also reduced the absolute slope (|m|) from 2.093 to 1.366. This reduction appears to indicate that the material continues to carry load rather than experiencing sudden failure at the moment of fracture, thereby acquiring ductile behavior.
Consequently, the FI values, summarized in
Figure 17, highlight the superior performance of the 7.5% Wiry mixture. This specific mixture achieved an FI of 24.17, representing an approximate 3.7-fold improvement over the control sample. This mechanism of increase is described in the literature as the “crack bridging” effect, where fibrous structures connect micro-cracks within the matrix, transferring stresses and delaying crack progression [
1,
16]. While “Random” geometry additives also enhanced performance, reaching a maximum FI of 11.94 at the 7.5% rate, they were not as effective as the “Wiry” type. This difference is attributed to the “Wiry” structure providing better interlocking with the aggregate matrix and more efficient load transfer. For both additive groups, 7.5% was identified as the optimum usage amount. When the additive rate was increased to 10% and 12.5%, a decline in FI values was observed; for example, the FI for 12.5% Wiry decreased to 13.65. This loss of performance at high rates is associated with the agglomeration of additives within the mixture and insufficient coating of aggregates by bitumen, leading to the formation of weak adherence zones [
49]. Similar studies have reported that excessive fiber/additive usage reduces workability and negatively affects air void distribution, thereby degrading mechanical performance [
50]. In conclusion, the use of 7.5% “Wiry” waste additive stands out as the most suitable modification to maximize the intermediate temperature cracking resistance of asphalt mixtures.
3.6. Cantabro Test Results and Evaluation
The Cantabro loss test was conducted to evaluate the resistance of the asphalt mixtures to disintegration and raveling under abrasive forces. The percentage of mass loss for the control and modified mixtures is presented in
Figure 18.
The results indicate a distinct divergence in performance governed by the geometric shape of the waste PVC additives. The control mixture exhibited a mass loss of approximately 7.6%. Upon analysis of the “Wiry” series, it is observed that the inclusion of fibrous PVC particles improved the durability of the mixture, reducing the mass loss to a minimum of 5.6% at the optimum content of 7.5%. This improvement is attributed to the reinforcement mechanism provided by the wire-like structures, which act as a three-dimensional network within the matrix, holding the aggregate particles together and preventing dislodgement during the tumbling process [
51]. Conversely, the “Random” series demonstrated a negative trend; as the content of random-shaped PVC increased, the mass loss rose significantly, reaching approximately 12.2% at the 12.5% substitution rate. This deterioration suggests that the non-fibrous, random particles may disrupt the interlocking of the aggregate skeleton and weaken the bitumen–aggregate adhesion, thereby making the mixture more susceptible to raveling [
42]. While the “Wiry” modification enhanced the resistance to abrasion, the excessive mass loss observed in high-content “Random” samples highlights the critical importance of additive geometry in maintaining the structural integrity of the asphalt surface course.
It should be noted that, although the Cantabro test is widely used for evaluating raveling resistance, its application to dense-graded asphalt mixtures remains limited, and no universally accepted specification limits are available for such mixtures. Previous studies have indicated that the Cantabro test can be used as a relative indicator of mixture durability rather than an absolute performance criterion. It is reported that mass loss values for dense-graded asphalt mixtures were generally below 15%, highlighting the potential of the test as a comparative evaluation tool rather than a specification-based acceptance method [
44]. In addition, the Cantabro test can also be effectively used to evaluate the mixing efficiency and dispersion quality of modifiers within dense-graded asphalt mixtures [
52].
In this context, the Cantabro results obtained in the present study (ranging approximately between 5% and 12%, as shown in
Figure 18) are consistent with the ranges reported in the literature for dense-graded mixtures. Therefore, the performance of the mixtures was assessed on a comparative basis, focusing on the relative differences between the control and PVC-modified mixtures. The results indicate that the use of wiry-shaped PVC additives leads to lower mass loss values compared to random-shaped particles, suggesting improved resistance to raveling. This behavior may also be associated with a more effective distribution and interaction of the wiry PVC within the mixture structure. However, these findings should be interpreted within the framework of relative performance evaluation, given the absence of standardized threshold values for dense-graded mixtures.
3.7. Statistical Evaluation of Experimental Results
Two-way analysis of variance (ANOVA) was performed to evaluate the effects of PVC geometry and additive content on the performance of asphalt mixtures. The results are summarized in
Table 9.
The analysis showed that both geometry and dosage had statistically significant effects on most performance parameters, including Cantabro loss, TSR, and FI (p < 0.05). Geometry appears to play a dominant role in rutting resistance (HWTT) and cracking resistance (FI), while dosage has a more pronounced influence on permanent deformation (RCT).
A significant interaction effect between geometry and dosage was observed for TSR and FI (p < 0.05), indicating that moisture susceptibility and cracking behavior are influenced by the combined effect of additive morphology and content. In contrast, Cantabro loss and HWTT results were primarily affected by independent contributions of these factors.
Following the ANOVA, post hoc comparisons were conducted to further examine the differences between mixture groups across all evaluated performance parameters. The results indicated that mixtures modified with wiry-shaped PVC generally exhibited superior performance compared to both control and random-modified mixtures, particularly for FI and TSR. Differences among mixture groups for Cantabro loss, HWTT, and RCT parameters were comparatively less pronounced.
These findings suggest that different performance mechanisms respond differently to PVC modification. Overall, the statistical analysis supports the experimental observations and indicates that optimum performance is observed at moderate additive contents, particularly for wiry-shaped PVC.
The experimental results identifying an optimum PVC content of 7.5% demonstrate a high degree of correlation with theoretical thresholds and practical benchmarks established in the literature. Previous studies on polymer-modified asphalt mixtures have indicated that plastic contents in the range of approximately 5–10% by weight of the binder provide an optimal balance between mechanical performance and workability [
7,
19]. Beyond this critical concentration, the excessive increase in kinematic viscosity often impedes the workability and compactability of the mixture, while simultaneously predisposing the pavement to low-temperature thermal cracking. Therefore, the 7.5% dosage achieved in this study represents an ideal equilibrium between maximizing the mechanical properties of asphalt mixtures.
Furthermore, the superior performance of the “wiry” (fibrous/slender) cutting geometry compared to “random” (granular) distribution can be elucidated through the reinforcement effect theory in composite materials. The elongated morphology of wiry PVC particles functions as a micro-reinforcing network within the aggregate–bitumen matrix, enhancing load transfer mechanisms and mitigating tensile stresses. A previous study [
53] suggests that a higher aspect ratio in polymer additives strengthens the interfacial adhesion between the binder and the aggregate, thereby increasing the cohesive resistance of the asphalt concrete. This morphological advantage explains the enhanced stiffness modulus and fatigue life observed in samples modified with wiry-cut waste.
The HWTT results indicate that the mixture containing 12.5% wiry PVC exhibited the lowest deformation and creep slope values, suggesting superior resistance to permanent deformation under water-submerged, high-temperature conditions. However, this observation differs from the outcomes of the other performance tests, where the optimum dosage was consistently identified as 7.5%. This discrepancy may be attributed to the intrinsic characteristics of the HWTT, which is performed under submerged conditions and simultaneously captures rutting and moisture-induced damage. The evolution of deformation in this test is governed not only by shear resistance, but also by changes in adhesion and cohesion within the mixture. While higher PVC contents may improve resistance to deformation through increased stiffness, they may also alter the binder–aggregate interaction and internal cohesion. Therefore, the coupled influence of moisture susceptibility and rutting behavior in the HWTT may lead to performance trends that differ from those observed in tests where these mechanisms are evaluated independently.
A general decline in the mechanical performance of asphalt mixtures was observed at higher PVC contents (10% and 12.5%). This deterioration may be attributed to the agglomeration of PVC particles at elevated dosages, which can negatively affect mixture homogeneity and internal structure. This behavior is further supported by the consistent deterioration observed in TSR, Cantabro loss, and creep performance at higher dosages. These combined trends indicate a loss of mixture homogeneity and the formation of weak zones within the asphalt matrix, which may be associated with particle agglomeration.
Although this study primarily focuses on the mechanical performance of waste PVC-modified asphalt mixtures, the use of waste-derived materials also presents potential environmental benefits. The incorporation of waste PVC foils can contribute to reducing plastic waste accumulation and support circular economy principles by diverting materials from landfills into infrastructure applications. In addition, partial replacement of conventional materials with waste-based additives may reduce the demand for virgin resources. However, the environmental implications of this approach were not quantitatively evaluated in this study; therefore, these benefits should be interpreted qualitatively. Potential limitations, including processing-related energy consumption and long-term environmental considerations, should also be acknowledged.
In addition to sustainability aspects, practical considerations such as workability, mixing uniformity, and field applicability should also be taken into account. The incorporation of waste PVC additives through the dry process may influence mixture handling and compaction behavior, depending on particle shape and content. In this study, the adopted mixing protocol provided a relatively homogeneous distribution of the additive, particularly for wiry-shaped PVC, which appeared to enhance interaction within the mixture structure. However, the potential for agglomeration, especially at higher additive contents or with irregular particle geometries, should be considered. From a practical perspective, the use of waste PVC is not expected to require significant modifications to conventional asphalt production processes; however, careful control of mixing conditions may be necessary to ensure uniform dispersion. Further investigation under plant and field conditions is recommended to confirm constructability and long-term performance.