Materials
The three asphalt binders selected in this study, as summarized in Table 1, are representative pavement binders derived from different crude oil sources and have been widely used in practical road engineering in China. Karamay asphalt, CNOOC 36-1 asphalt, and PetroChina asphalt differ markedly in crude origin, chemical composition, aging susceptibility, and rheological characteristics, providing a suitable material basis for investigating oil-source-dependent fatigue behavior. Their selection enables a comparative evaluation of how intrinsic binder composition influences the effectiveness of warm-mix modification and mixture-scale fatigue performance, thereby enhancing the engineering relevance of the proposed cross-scale fatigue characterization framework. Detailed geological origins and chemical characteristics of each binder are as follows:
Binder A: Derived from heavy oil feedstock of the 9th zone, produced via a blending process of vacuum residue and deoiled asphalt. Its base material exhibits distinctive properties, including low paraffin content (<2%), minimal sulfur concentration, and high resin composition. Notably, Karamay asphalt is the only pavement binder with a specific gravity below 1 g/cm3 in current engineering applications, and it features superior dynamic viscosity and excellent ductility retention after aging. These characteristics make it particularly suitable for regions subjected to large diurnal temperature variations and intense ultraviolet exposure.
Binder B: Originates from the rare heavy crude oil extracted from the Suizhong 36-1 offshore oilfield, with a high bitumen yield of 56% through refining. The feedstock is classified as a sulfur-deficient, naphthenic-base heavy crude with a high acid value, resulting in a processed binder with high density (1.012 g/cm3), low paraffin content (1.8%), and elevated resin proportions. Such properties endow the binder with excellent low-temperature flexibility, rendering it advantageous for cold environment applications.
Binder C: Primarily formulated using Venezuelan Boscan heavy crude as the base feedstock, achieving a 60% production yield via specialized refining processes. This crude oil exhibits unique geochemical features, including high acid content, significant heavy metal concentrations, and strong carbon residue formation potential. The binder displays an atypical hydrocarbon composition, characterized by low saturated hydrocarbon fractions, enriched resin-asphaltene complexes, and remarkably low paraffin content (1.3%).
In this investigation, the three base asphalt binders were designated as AO (Karamay), BO (CNOOC 36-1), and CO (PetroChina). Corresponding WMA binders were prepared by incorporating Evotherm M1 additive, coded as AP, BP, and CP, respectively20. Comprehensive performance indices, including penetration, softening point, and ductility, were tested in accordance with JTG E20-201121 specifications, with detailed comparative data presented in Table 1. All experimental procedures were strictly followed by the standardized protocols outlined in the Technical Specifications for Highway Engineering Asphalt and Bituminous Mixtures.
| Project | Unit | Karamay | CNOOC | CNPC |
| Penetration | 0.1 mm (15 °C) | 22 | 22 | 24 |
| 0.1 mm (25 °C) | 72 | 68 | 71 |
| 0.1 mm (30 °C) | 112 | 110 | 116 |
| PI | - | -1.14 | -1.2 | -0.81 |
| TR&B | °C | 46 | 46.5 | 47.5 |
| Dynamic viscosity (60 °C) | Pa·s | 223.5 | 230 | 256.9 |
| Ductility (10 °C,5 cm/min) | cm | >100 | >100 | 52 |
| Wax content | % | 1.9 | 1.8 | 1.3 |
| Flash point (COC) | ℃ | 278 | 287 | 312 |
| Solubility | % | 99.5 | 99.7 | 99.8 |
| Density (15 °C) | g/cm³ | 0.977 | 1.012 | 1.049 |
| RTFOT | Quality change (%) | 0.05 | 0.06 | -0.07 |
| Residual penetration ratio (%) | 66.2 | 67.4 | 64.8 |
| Residual ductility (10 °C,cm) | 13 | 12 | 9 |
Table 1: Key technical parameters of bituminous binders. Table 1 summarizes the key technical parameters of bituminous binders, including physical properties, temperature susceptibility, rheological characteristics, and short-term aging performance, to evaluate their fundamental properties and durability.
The WMA preparation process involved a strictly controlled multi-stage protocol designed to ensure reproducibility of binder modification. The base asphalt binder was first heated in a forced-convection oven at 135 ± 2 °C for 60 min to achieve a stable molten state, followed by 30 min of equilibration to eliminate thermal gradients. All heating processes were conducted under sealed containers with nitrogen protection (flow rate: 0.5 L/min) to minimize oxidative aging during temperature conditioning.
The Evotherm M1 additive was then incorporated at 135 ± 2 °C under continuous mechanical stirring at 300 rpm for 5 min prior to high-shear processing, ensuring initial dispersion of the surfactant phase. Subsequently, high-shear mixing was performed using a rotor–stator homogenizer at 3000 rpm for 25 min, while maintaining the binder temperature within 135–140 °C using an external oil bath temperature control system (±1 °C accuracy). During the entire mixing process, the temperature was continuously monitored using a calibrated K-type thermocouple inserted into the binder matrix, and fluctuations exceeding ±2 °C triggered automatic heating adjustment. The modified binder was then subjected to a controlled cooling procedure to 25 °C at 5 °C/min before subsequent testing or short-term storage. The shear protocol design followed the viscosity–temperature relationship of asphalt binders, ensuring that all samples were prepared under comparable shear history conditions. This strict thermal–mechanical control guarantees high repeatability and minimizes variability in WMA binder preparation.
Dynamic shear rheometer (DSR) testing
To characterize the rheological response and fatigue-related properties of asphalt binders modified with warm-mix additives, Dynamic shear rheometer (DSR) tests were conducted using a temperature-controlled rotational rheometer in accordance with ASTM D717522. The rheological evaluation focused on intermediate-temperature fatigue behavior, which is closely associated with crack initiation and propagation in asphalt pavements.
The fatigue factor G*sin δ23, widely recognized as an indicator of fatigue susceptibility at the binder level, was adopted to quantify changes in viscoelastic dissipation behavior induced by warm-mix modification and aging. Temperature sweep tests were performed over a range of 58–82 °C, with temperature increments of 6 °C. At each target temperature, specimens were allowed to equilibrate for 10 min before data acquisition to ensure thermal stability. To investigate the influence of aging on rheological properties, binder specimens were subjected to three aging conditions: unaged, rolling thin film oven test (RTFOT) aging, and combined RTFOT and Pressure Aging Vessel (PAV) aging 24. These aging protocols were designed to simulate short-term aging during production and placement, as well as long-term aging during in-service pavement operation. The evolution of G*sin δ with temperature and aging condition was analyzed to assess the fatigue resistance of different binders.
Before each DSR test, the binder specimen was carefully trimmed after loading between the parallel plates to ensure a uniform edge profile. The specimen was conditioned at the target temperature for 10 min before measurement. Testing was performed over 58–82 °C at 6 °C increments. A valid test was confirmed when the measured torque and displacement remained within the instrument’s recommended operating range, and no visible specimen slippage occurred.
Linear amplitude sweep (LAS) testing
Viscoelastic behavior characterization was conducted in accordance with ASTM D7175 specifications for dynamic mechanical analysis25. The experimental methodology included strain amplitude sweeps to establish linear viscoelastic boundaries, followed by frequency-controlled testing at 10 rad/s26. Temperature-dependent evaluations covered the operational temperature spectrum of asphalt pavements (58–82°C), executed in 6°C increments with 10 minutes allowed for thermal equilibrium at each isothermal segment. The AASHTO T391 protocol was employed to quantify binder damage accumulation through dissipated energy evolution, specifically monitoring the viscoelastic dissipation factor (|G*|sin δ) during cyclic loading 27,28. The Simplified Viscoelastic Continuum Damage (S-VECD) framework was adopted to predict degradation patterns of bituminous composites29. The LAS protocol executes an oscillatory amplitude sweep at a fixed 10 Hz frequency, applying controlled strain progression from 0.1% to 30% with 0.1% resolution increments.
Key viscoelastic parameters were derived using the following equations:
log G "(ω) = m (log ω) + b (1)
G'(ω) = G* (ω) × cosδ (ω) (2)
(3)
where G''(ω) is the loss modulus, ω is the angular frequency, m and b are fitting coefficients, G'(ω) is the storage modulus, G*(ω) is the complex modulus, δ(ω) is the phase angle, and is the viscoelasticity index.
Damage quantification employed the fundamental relationship expressed in Equation (4):
(4)
In the formula: C(t)—the integrity parameter, C(t)=G^* (t)/G^* (Initial), G^*- complex modulus (MPa);
γ_0—Applying strain (%);
t—Test duration (s)
The temporal evolution of damage metric D(t) and structural integrity coefficient C(t) is mathematically parameterized through a power-law constitutive relationship (Yuan 2024):
C(t) = C0 - C1 × DC2 (5)
In the formula: C0 represents the initial integrity parameter (normally equal to 1) ,C1, C2—fitting parameters.
Calculate the fatigue damage value using the concept of the shear stress peak point:
(6)
Cpeak is the integrity parameter corresponding to the maximum shear stress point.
The fatigue life calculation formula is:
Nf = A(γmax)-B (7)
In the formula: A, B—fatigue-related coefficient,
A = f × (Df)[1 + (1 - C2 )a] / {[1 + (1 - C2 )a] × (πC1 C2 )a} (8)
B=2a, f-loading frequency;
γmax — expected maximum strain level (%)
To ensure the reliability and reproducibility of experimental results, all binder-scale and mixture-scale tests were conducted with at least 3 independent replicates (n = 3) per condition. The reported results represent the mean values of replicate measurements. The variability of experimental data was evaluated using standard deviation (SD), and error bars are provided in all relevant figures to reflect statistical dispersion. For LAS–S-VECD parameters, DSR rheological indices, and fatigue life from four-point bending tests, the coefficient of variation (COV) was additionally calculated to assess data consistency.
In all cases, statistical differences between modified and unmodified binders were examined to ensure that observed trends are not due to experimental scatter but represent statistically meaningful differences in fatigue and rheological behavior.
Four-point bending fatique testing
To validate binder-level fatigue indicators and establish cross-scale correlations, four-point bending fatigue tests were conducted on asphalt mixtures prepared using an AC-16C gradation30,31. The aggregate gradation, apparent density, bulk specific gravity, and water absorption of each aggregate size, together with the properties of the mineral filler, are summarized in Table 2. The asphalt content of all mixtures was fixed at 4.8% to ensure consistency across different WMA formulations.
| Sieve Size (mm) | Aggregate Category | Synthetic Grading (%) |
| 1# (10~20mm. 29%) | 2# (5~10mm. 29.2%) | 3# (3~5mm. 17%) | 4# (0~3mm. 19%) | Mineral Powder (5.8%) | |
| 0.075 | 0 | 0.1 | 0 | 0.9 | 90.8 | 5.5 |
| 0.15 | 0.1 | 0.1 | 0 | 4.9 | 95.3 | 6.5 |
| 0.3 | 0.1 | 0.2 | 0 | 13 | 98.7 | 8.3 |
| 0.6 | 0.1 | 0.2 | 0 | 25.2 | 99.7 | 10.6 |
| 1.18 | 0.1 | 0.2 | 0 | 47.8 | 100 | 15 |
| 2.36 | 0.1 | 0.5 | 0 | 100 | 100 | 25 |
| 4.75 | 0.8 | 15.5 | 98.9 | 100 | 100 | 46.4 |
| 9.5 | 15.2 | 99.5 | 100 | 100 | 100 | 75.2 |
| 13.2 | 68.4 | 99.8 | 100 | 100 | 100 | 90.8 |
| 16 | 94.8 | 100 | 100 | 100 | 100 | 98.5 |
| 19 | 100 | 100 | 100 | 100 | 100 | 100 |
| Apparent Relative Density | 2.899 | 2.918 | 2.845 | 2.754 | 2.872 | 2.865 |
| SSD Relative Density | 2.854 | 2.847 | 2.816 | 2.691 | - | 2.814 |
| Bulk Specific Gravity | 2.829 | 2.81 | 2.8 | 2.655 | - | 2.787 |
| Aggregate Water Absorption Rate (%) | 0.85 | 1.32 | 0.56 | 1.36 | - | - |
Table 2: Grading of aggregates in warm-mix asphalt mixture. Table 2 presents the aggregate gradation of the warm-mix asphalt mixture, including the proportions of different aggregate fractions, mineral powder content, synthetic gradation curve, and aggregate physical properties. The table presents the designed particle-size distribution and the basic characteristics of the aggregates used in the asphalt mixture.
Four-point bending fatigue tests were performed using a Cooper testing apparatus under strain-controlled loading conditions to evaluate the fatigue durability of warm-mix asphalt (WMA) mixtures32. The failure criterion was defined as the number of loading cycles required for the flexural stiffness to decrease to 50% of its initial value. In accordance with the established testing protocol33, cyclic loading was applied in the form of a continuous sinusoidal waveform at a frequency of 10 Hz under isothermal conditions of 15 °C. All tests were conducted without rest periods to ensure uninterrupted energy input during fatigue loading34,35.
Beam specimens were fabricated in accordance with standard dimensional requirements, with a length of 381 ± 6.35 mm, a width of 63.5 ± 6.35 mm, and a height of 50.8 ± 6.35 mm3637. Under strain-controlled conditions, fatigue performance was characterized by plotting fatigue characteristic curves for specimens with different WMA formulations in a double-logarithmic coordinate system38. A power-law constitutive relationship was subsequently established, and nonlinear regression analysis was employed to fit the fatigue data of the various asphalt mixtures, providing the basis for subsequent fatigue life modeling and comparative analysis39,40,41. The beam specimen was mounted symmetrically in the four-point bending fixture, and contact between the loading clamps and specimen surface was checked before loading. The test was conducted at 15 °C under strain-controlled sinusoidal loading at 10 Hz without rest periods. The test endpoint was defined as the number of cycles at which flexural stiffness decreased to 50% of its initial value. Tests were considered valid when failure occurred within the gauge section, and no abnormal clamp slippage or sudden non-fatigue fracture was observed. All quantitative data are presented as mean ± standard deviation (mean ± SD), with sample size n = 3 for all experimental groups unless otherwise specified.