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ORIGINAL RESEARCH article

Front. Mater., 14 January 2026

Sec. Smart Materials

Volume 12 - 2025 | https://doi.org/10.3389/fmats.2025.1758696

This article is part of the Research TopicFunctional Materials for Sustainable Pavement Engineering: Multi-scale Design and Environmental IntegrationView all 9 articles

Study on the physical properties, anti-aging properties, and rheological characteristics of graphene oxide/rubber powder composite modified asphalt

Youtao WangYoutao Wang1Yongzhen SunYongzhen Sun1Lujie HuangLujie Huang1Xiaofeng WangXiaofeng Wang1Chanyuan Lin
Chanyuan Lin2*
  • 1China Railway First Group Third Engineering Co., Ltd., Baoji, Shanxi, China
  • 2College of Civil Engineering and Architecture, Guangxi University, Nanning, China

Introduction: The goal of this project is to enhance the construction operability, durability, aging resistance, and high-temperature performance of crumb rubber modified asphalt (CRMA) while encouraging tire recycling in order to meet environmental goals.

Methods: To this end, graphene oxide (GO) is incorporated into the CRMA system to form a GO-CRMA composite material. The modification effects of this composite will be systematically investigated, with the goal of developing a high-performance composite modified asphalt that exhibits outstanding road performance and significant environmental benefits. 70 penetration grade asphalt was selected as the base asphalt (BA); 20% (by mass of BA) crumb rubber was introduced together with GO at dosages of 0.3%, 0.6%, 0.9% and 1.2% (by mass of BA) to produce graphene-oxide/crumb-rubber composite-modified asphalt (GOR). Penetration, softening point, ductility, Brookfield rotational viscosity, and segregation experiments were employed to evaluate physical properties; laboratory simulated aging tests were implemented to evaluate anti-aging performance by analyzing retained-penetration ratio and softening-point increment; and a temperature sweep test revealed high-temperature rheological characteristics of GOR by examining rheological variables like complex modulus (G*), phase angle (δ), and rutting factor (G*/sinδ).

Results: Results show that at a GO dosage of 0.3% the GOR reaches a softening point of 66.3 °C, a ductility 6.9% higher than that of CRMA, a Brookfield viscosity 5% lower, and the minimum segregation softening-point difference; After ageing, it shows the highest level of residual penetration and the lowest softening-point increment; G* and G*/sinδ increase significantly while δ decreases, indicating the best high-temperature rheological performance.

Discussion: In summary, incorporating an appropriate amount of GO can effectively enhance the overall performance of CRMA, with 0.3% identified as the optimal dosage, demonstrating promising prospects for engineering applications.

1 Introduction

Approximately 1.4 billion tires are used annually due to the fast growth of the global automotive industry and the ongoing rise in the number of cars in use, which results in an increasing amount of waste rubber tires (Li et al., 2022; Liu and Gu, 2025). Rubber materials exhibit high thermal stability and resistance to degradation; improper disposal therefore triggers multiple environmental problems. On the one hand, combustion releases large quantities of harmful gases and carbon monoxide, causing atmospheric pollution. On the other hand, tire rubber is a refractory high-molecular-weight elastomer that possesses outstanding resistance to heat, mechanical stress and corrosion. Consequently, it is extremely recalcitrant to degradation in the natural environment, and discarded tires can persist for decades or even centuries under natural conditions, posing long-term hazards to the environment (Liu et al., 2024).

According to earlier research, crumb rubber made from used tires can be applied as a modifier when making CRMA. The approach not only leverages the elasticity and flexibility of rubber to enhance asphalt performance but also facilitates the resource utilization of discarded tires (Su et al., 2024). Using waste rubber powder in road construction offers a broad and low-cost raw material source, effectively reducing project costs. This strategy supports China’s development objectives of creating an ecologically conscious and resource-conserving society, while also enabling efficient recycling of waste. It delivers both significant economic and environmental benefits (Li H. et al., 2024). Consequently, this technology is finding ever-wider application in road engineering. The characteristics of CRMA have previously been the subject of numerous researches. Zhang et al. (2024) examined how crumb rubber affected the rheological characteristics of asphalt; Hoy et al. (2024), Huang J. et al. (2024) investigated the fatigue performance of CRMA mixtures; Cai et al. (2025) systematically evaluated how key parameters of crumb rubber (CR), namely, particle size and content, affect the asphalt’s high-temperature rheological behavior. Nevertheless, CRMA still faces challenges in practical engineering applications. On the one hand, the viscosity of CRMA is directly correlated with CR content, with higher dosages leading to elevated viscosity levels., which tends to reduce mixture workability, increases construction difficulty, and affects pavement smoothness and compaction quality (Li K. et al., 2024; Yu et al., 2020; Zhao et al., 2024). However, the material CRMA’s storage stability throughout construction and transit is likewise inadequate (Huang W. et al., 2024). Therefore, further research and improvement in the preparation and construction technologies of CRMA are essential to enhance its workability and storage stability, thereby ensuring that its advantages in road engineering can be fully realized.

Graphene oxide (GO) is a novel nanomaterial with exceptional physicochemical properties and high mechanical strength, characterized by a large specific surface area and excellent dispersibility (Yang et al., 2024). These attributes have made GO a nanomaterial of great interest and promise in asphalt technology. Unlike many nanomaterials that can only enhance a single property of asphalt, GO—with its uniqueness combination of structure and chemistry—delivers balanced improvements in mechanical performance, high-temperature stability, and durability (Peng et al., 2025). In addition, GO encourages a stable colloidal structure and a more uniform component distribution, thereby enhancing asphalt’s toughness, adhesion, and resistance to ageing. (Li et al., 2025).

Therefore, this study intends to use rubber powder prepared from waste tires and GO as asphalt modifiers to systematically investigate the impact of different GO dosages on the performance of CRMA. With penetration, ductility, softening-point, Brookfield rotational-viscosity and segregation tests, the physical properties of the GOR will be systematically evaluated. Indoor simulated aging tests will be conducted, and indices such as retained penetration and softening-point increment will be adopted to assess its aging resistance. Additionally, dynamic temperature-sweep tests will be conducted to examine GOR’s high-temperature rheological properties. The aim of this work is to develop an innovation approach for the resource utilization of waste tires, which holds significant importance for promoting environmental protection and green development.

2 Materials and methods

2.1 Materials

2.1.1 Base asphalt

In this work, 70 penetration grade asphalt was employed as the BA. Its fundamental properties were tested in accordance with the JTG 3410-2025; the findings, listed in Table 1, fully comply with the specification requirements.

Table 1
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Table 1. Technical requirements for BA.

2.1.2 Graphene oxide

The graphene oxide (GO) utilized in this investigation is depicted in Figure 1 and Table 2 lists its technical parameters.

Figure 1
A pile of black powder on a flat, light-colored surface. The powder is loosely spread, with finer particles scattered around the edges of the main pile.

Figure 1. Appearance of graphene oxide.

Table 2
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Table 2. Graphene oxide parameters.

2.1.3 Crumb rubber

Table 3 displays the typical properties of the CR particles used for this work, which have a size of 60 mesh (see Figure 2).

Table 3
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Table 3. Technical indicators of CR.

Figure 2
A pile of finely ground black powder on a light surface, with some stray particles scattered around the edges.

Figure 2. Appearance of crumb rubber.

2.2 Methods

2.2.1 Preparation of modified asphalt

This study adopts the following pretreatment process: CR and GO dehydrate in an oven at 120 °C for 1h, and the BA then heated at 135 °C until it reaches a molten, flowable state, thereby preventing the formation of numerous bubbles when the modifiers are blended with the asphalt under high temperature. According to existing relevant research (Li L.et al., 2024), the size effect of GO hinders CR from absorbing light components, and CR will further increase its specific surface area after being sheared, making it difficult to disperse in asphalt. Therefore, GO is first dispersed in the asphalt before CR is added. Figure 3 depicts the preparation procedure.

Figure 3
A schematic diagram showing a processing sequence. First, a beaker labeled

Figure 3. Preparation process of GOR.

The detailed preparation the program is as follows: (1) Weigh 500 g of the base asphalt in the molten state into a beaker and heat it to 180 °C on a hot plate. (2) Add GO at 0.3%, 0.6%, 0.9% and 1.2% by mass of asphalt, then manually stir by a rod for 5 min until the GO is dispersed and no visible agglomerates remain. The determination of the 0.3%–1.2% GO dosage range was based on the results of pre-experimental studies. When the GO dosage was below 0.3%, it did not exhibit a significant impact on the properties of CRMA. (3) Introduce 20% CR by mass of BA and subject the blend to shearing at 1,000 r/min for 15 min to eliminate bubbles and obtain a uniform pre-dispersion; subsequently shear at 5,000 r/min at 180 °C for 1 h. (4) After shearing, condition the sample in a 180 °C oven for 1 h to allow swelling and development, yielding the final GOR. In parallel, a control CRMA containing 20% CR (without GO) is prepared by an identical protocol.

2.2.2 Laboratory simulated aging test

Asphalt-Aging that occurs during service life may have a important impact on the performance of asphalt mixtures (Hou et al., 2018). Short-term aging (STA) primarily occurs during the construction phase—i.e., while the mix is being produced, transported and laid—whereas long-term aging takes place progressively throughout the pavement’s service life under sustained environmental exposure. The pavement’s service life is when long-term aging (LTA) mostly happens, developing gradually under sustained environmental exposure. The aging experienced by different asphalt asphalts during construction and in-service periods can be simulated by means of the Pressure Aging Vessel (PAV) for LTA and the Rolling Thin-Film Oven Test (RTFOT) for STA (Tian et al., 2021). Consequently, this study employs a CS325-B subjecting the various asphalt samples to STA and LTA in a rotary thin-film oven and a pressure-aging vessel, respectively., thereby evaluating the aging resistance of CRMA and GOR.

2.2.3 Physical performance testing of composite-modified asphalt

In compliance with the Chinese standard JTG 3410-2025, this study evaluated the asphalt’s physical performance for penetration, ductility, softening-point, Brookfield rotational-viscosity, and segregation.

2.2.4 Dynamic temperature sweep test

To examine the high-temperature rheological behavior of the asphalts, the dynamic shear rheometer was used to demonstrate dynamic temperature-sweep tests for different asphalt samples in this research. By analyzing indicators such as the δ and G* of samples, the high-temperature rheological performance of the asphalt can be assessed. During the test, the water bath temperature range was established at 34 °C–82 °C., with a temperature interval of 6 °C. The parallel plate diameter used in the test was 25 mm, the parallel plate spacing was maintained at 1 mm, the strain was controlled at 1%, with the test loading frequency was set at 1.59 Hz to keep the asphalt samples where the material exhibits linear viscoelastic behaviour.

3 Results and discussion

3.1 Analysis of physical performance test results of composite-modified asphalt

3.1.1 Softening point

The softening point test results for the asphalt samples are presented in Figure 4. Figure 4 shows the softening point test results of different asphalt samples. The softening point of CRMA is 63.5 °C. For GOR, when the GO content is 0.3%, 0.6%, 0.9%, and 1.2%, the corresponding softening points are 66.3 °C, 65.6 °C, 65.2 °C, and 65.0 °C, respectively. At a GO dosage of 0.3% the softening point rises most markedly and reaches its maximum; with further GO addition the value decreases slightly. The higher softening point of GOR indicates improved high-temperature stability and lower temperature susceptibility. This can be ascribed to the high density of surface oxygen-containing functional groups of GO, which interact with organic molecules in the asphalt to establish a stable network that effectively restrains molecular mobility at elevated temperatures, thereby leading to a rise in the softening point and an enhancement in the high-temperature performance of GOR.

Figure 4
Bar chart showing the softening point in degrees Celsius of various asphalt samples: CR at 63°C, 0.3GOR at 66°C, 0.6GOR at 65°C, 0.9GOR at 64.5°C, and 1.2GOR at 64°C. Error bars are present.

Figure 4. Results of softening points of different asphalt samples.

3.1.2 Penetration

The results of penetration tests are plotted in Figure 5. The CRMA registered 44.8 (0.1 mm); after GO was introduced the penetration values of GOR decreased, but the reduction was modest, indicating that GO addition raises the consistency of CRMA. At a GO dosage of 0.3% the penetration of GOR reaches its minimum; with further GO addition the penetration increases slightly, but the variation remains small, demonstrating that GO does not exert a pronounced influence on the consistency of CRMA.

Figure 5
Bar chart comparing penetration of various asphalt samples in units of 0.1 millimeters. Samples include CR, 0.3 GOR, 0.6 GOR, 0.9 GOR, and 1.2 GOR. Penetration values range from approximately 41 to 45. Error bars indicate variability, and a line connects the tops of the bars.

Figure 5. The penetration test results of different asphalt samples.

3.1.3 Ductility

Ductility testing was used in this study to assess the asphalt’s performance at low temperatures. The test was carried out at a constant temperature of 5 °C with a constant pulling speed of 1 cm/min. The test results are summarized in Figure 6.

Figure 6
Chart showing ductility of asphalt samples: CR, 0.3GOR, 0.6GOR, 0.9GOR, and 1.2GOR. Ductility is measured in centimeters, ranging from 10.7 for CR to 9.3 for 1.2GOR. Error bars and a connecting line indicate variations.

Figure 6. The ductility test results of different asphalt specimens.

The initial increase followed by a decline in the asphalt’s ductility, which dropped from 10.2 cm to 9.3 cm with GO addition, is illustrated in Figure 6. At a GO dosage of 0.3% the ductility reaches 10.8 cm, 6.9% higher than that of CRMA. As the GO content rises from 0.3% to 1.2% the ductility falls continuously, dropping 8.3%, 12% and 13.9% below the CRMA value, respectively. This indicates that a low GO content can boost the low-temperature crack resistance of CRMA. The reason lies in the physical dispersion and interfacial strengthening provided by GO: its lamellae are uniformly distributed throughout the CRMA, building a stable network that effectively disperses stresses and enhances interfacial bonding, thereby increasing the toughness and extensibility of the asphalt. As the GO dosage continues to increase, agglomeration tends to occur, producing larger particles or slip planes. These agglomerates not only disrupt the uniformly dispersed network but also impede the movement of asphalt molecules, suppressing stress relaxation and thus degrading low-temperature cracking resistance.

3.1.4 Brookfield rotational viscosity

Asphalt viscosity correlates strongly with its rheological properties and, to a considerable extent, indicates the asphalt’s resistance to shear deformation. At elevated temperatures CR particles interact with and incorporate the light oil fractions of the asphalt., swell in volume and consequently undergo a swelling phenomenon. This process markedly reduces the light fractions that are free to flow within the asphalt, thereby increasing its viscosity (Zheng et al., 2021). From a construction perspective, an excessively high viscosity impairs the workability of the asphalt mixture, raising the difficulty of mixing, paving and compaction and thereby exerting an adverse effect on construction; consequently, The asphalt’s viscosity needs to be regulated within a certain range (Yang et al., 2020). The viscosity of the different asphalt samples measured at 180 °C in this study are shown in Figure 7.

Figure 7
Bar chart showing rotational viscosity (in milliPascal-seconds) for asphalt samples labeled CR, 0.3 GOR, 0.6 GOR, 0.9 GOR, and 1.2 GOR. Viscosity decreases from approximately 2200 to 1900 milliPascal-seconds. Annotations indicate viscosity differences of 113, 239, 256, and 318.

Figure 7. Results of rotational viscosity of different asphalt samples.

Figure 7 GO is effective in lowering the viscosity of asphalt, and as the GO dosage increases, the viscosity of the GOR shows a continuous downward trend. As the GO dosage rose from 0.3% to 1.2%, the viscosity of GOR fell 5%, 10.6%, 11.4% and 14.1% below that of CRMA, respectively. The reduction is attributed to the two-dimensional lamellar the structure of GO, which features abundant oxygen-containing functional groups, which adsorb polar fractions in the asphalt and weaken the physical entanglement among asphalt molecules, thereby lowering internal frictional resistance. Moreover, the uniformly dispersed GO sheets form a dense adsorption layer at the interface between CR molecular chains and the asphalt phase; this “lubricating skeleton” facilitates directional slippage of molecular chains under shear and thus further reduces the overall viscosity.

3.1.5 Storage stability

Considering the segregation of CRMA during storage, transportation, and construction, its performance can be significantly affected, thereby influencing its practical application effectiveness (Wen et al., 2020). Therefore, a segregation test was conducted to measure the softening-point difference between CRMA and GOR, to investigate the effect of varying GO contents regarding the storage stability of CRMA (Shatanawi et al., 2012) Figure 8 shows the test results.

Figure 8
Bar and line graph showing asphalt samples CR and various GOR levels. Bars represent softening points for Top (green) and Bottom (orange) sections in degrees Celsius. A line graph overlays with softening spread values. Error bars are included.

Figure 8. The segregation test results of different asphalt samples.

The significant softening-point difference of 5.5 °C between the upper (62.5 °C) and lower (68 °C) sections of CRMA, as depicted in Figure 8, is clear evidence of its poor storage stability. This is because CR particles engulf the light fractions of the asphalt and subsequently swell; the swollen CR then settles during prolonged standing, leading to phase separation at high temperatures and thus lowering storage stability. At all GO dosages, the softening-point difference of GOR is less than that of CRMA, and the difference first declines and then rises as the GO content rises. When 0.3% GO is added, the softening-point difference reaches its minimum, showing that the adding of a suitable amount of GO results in improved storage stability of CRMA, with 0.3% GO giving the best improvement. When 0.3% GO is incorporated, the top-bottom softening point difference of the asphalt sample reaches its minimum, demonstrating that an appropriate GO content can lead to a notable enhancement in the storage stability of CRMA and that 0.3% GO provides the best enhancement. This improvement stems from GO’s substantial specific surface area and surface energy, which enable asphalt molecules to adsorb stably onto its sheets. Meanwhile, the oxygen-bearing functional groups of GO can form chemical bonds with polar moieties in both CR and the asphalt matrix, suppressing chain scission of CR and breakdown of the cross-linked network. In doing so, GO effectively restrains the migration and agglomeration of This interaction between CR and asphalt molecules contributes to the enhanced storage stability of the modified asphalt.

3.2 Analysis of anti-aging performance test results

3.2.1 Retained penetration ratio

The retained-penetration ratio reflects the consistency change of asphalt before and after aging. A higher retained penetration ratio illustrated better aging resistance. Equation (1) can be used to determine the retained-penetration ratios of various asphalt samples.

KP=P2P1×100(1)

Where: Kp the ratio of the penetration of asphalt after aging, %.

P1 Penetration before testing, 0.1 mm.

P2 Penetration after testing, 0.1 mm.

The retained penetration ratios of the various asphalt asphalts after aging are presented in Figure 9.

Figure 9
Bar graphs comparing residual penetration percentages for different asphalt samples, labeled CR, 0.3 GOR, 0.6 GOR, 0.9 GOR, and 1.2 GOR. Graph (a) shows higher residual penetration percentages, ranging from 80.13% to 83.88%. Graph (b) shows lower percentages, ranging from 53.79% to 66.36%. Error bars indicate variability.

Figure 9. Residual penetration of different asphalt samples, (a) short-term, (b) long-term.

Figure 9 shows that the retained penetration of all asphalts decreased after both RTFOT and PAV aging. The results following STA are much higher than those following LTA, suggesting that the penetration decline increases with the length of the aging period, thus, the fluidity of the asphalt is more severely affected by prolonged aging. As illustrated in Figure 9a, after short-term aging the retained penetration of GOR is higher than that of CRMA, demonstrating that GO addition reduces the penetration loss caused by aging and thus improves the aging resistance of CRMA. With increasing GO content the retained penetration first rises and then falls, reaching its maximum of 83.88% at a GO dosage of 0.3%. This behavior arises because, during aging, the volatilization of light oil fractions and the oxidation reactions that occur when asphalt is exposed to air alter the molecular structure of the asphalt. Once the GO sheets are well-dispersed within the CR-modified asphalt they create an intercalated structure that acts as a physical barrier, hindering oxygen diffusion and retarding both the evaporation of light components and oxidative cross-linking reactions, thereby enhancing the asphalt’s aging resistance. As the GO content continues to increase, the retained-penetration ratio gradually declines. This is chiefly because excess GO agglomerates within the asphalt, weakening the effective interaction between GO and the asphalt constituents and reducing its ability to restrict molecular mobility; consequently, oxidative reactions and the loss of light fractions during aging are accelerated. Figure 9b reveals that after LTA the retained-penetration ratio follows the same trend observed after short-term aging: the ratio first increases and then decreases with GO content, peaking at 66.36% for the 0.3% GO dosage. This consistency confirms that incorporating 0.3% GO significantly enhances the ability of the asphalt to withstand long-term aging.

3.2.2 Softening point increment

A larger softening-point increment indicates a higher degree of aging that the asphalt has undergone during service. In this work, the softening-point increment of different asphalt samples after STA and LTA can be calculated using Equation 2.

ΔT=T2T1(2)

Where: Δ T Increase in softening point,° C.

T1 Softening point of asphalt sample prior to testing,° C.

T 2 Softening point of asphalt sample following the test,° C.

Figure 10 presents the softening point increments of the various samples after aging.

Figure 10
Bar charts labeled (a) and (b) compare the softening point increase in degrees Celsius for different asphalt samples: CR, 0.3 GOR, 0.6 GOR, 0.9 GOR, and 1.2 GOR. Chart (a) shows increases ranging from 1.8 to 2.9 degrees, while chart (b) shows increases from 1.5 to 3.8 degrees, demonstrating a trend of increasing softening point with higher GOR values.

Figure 10. The increments of softening points of five kinds of asphalt samples, (a) short-term, (b) long-term.

The findings demonstrate that all asphalt samples’ softening points rose to varied degrees following both RTFOT and PAV aging. The stems from the loss of light components through volatilization and their conversion into heavier fractions during ageing as well as the oxidation of asphalt upon exposure to oxygen, which generates polar molecules and enhances intermolecular forces, thereby raising the softening point. The softening point increments of the GOR blends are 4.8 °C, 5.1 °C, 5.4 °C and 5.9 °C as the GO dosage increases in Figure 10a. At 0.3% GO the increment is 2.9 °C lower than that of CRMA, indicating superior aging resistance. This is because GO reduces the amount of easily aging components in the asphalt by adsorbing its light components, while its lamellar structure blocks direct contact between oxygen and asphalt molecules and restrains molecular displacement, thereby enhancing intermolecular forces and retarding asphalt aging. Figure 10b reveals that the softening-point increment follows the same trend after both STA and LTA, the rise being more pronounced under long-term conditions. Compared with CRMA, the long-term increment of GOR is reduced at every GO level; the 0.3% GOR blend exhibits an increment of 11.8 °C, lower than that of CRMA and representing the largest reduction between any two asphalts. This indicates that GO also successfully increases the asphalt’s resilience to long-term aging, with the greatest improvement occurring at a dosage of 0.3%.

3.3 Rheological performance analysis

3.3.1 Complex modulus

The complex modulus G* serves as an indicator of the asphalt’s deformation resistance under dynamic shear. A higher complex modulus G* indicates that the asphalt possesses greater deformation resistance under load and that the proportion of its elastic component has been optimized (Chen M. et al., 2021). This study measured G* for all asphalt blends. Figure 11 displays the outcomes.

Figure 11
Graph showing the relationship between dynamic shear modulus (Pa) and temperature (°C). Several curves represent different GORs (Gas-Oil Ratios) and CR (Control Ratio) conditions. The y-axis measures dynamic shear modulus from 0 to 2 x 10^5 Pa, while the x-axis measures temperature from 34°C to 82°C. A zoomed-in section highlights data between 58°C and 59°C. Each curve is labeled with markers and colors: diamonds for CR, squares for 0.3 GOR, circles for 0.6 GOR, triangles for 0.9 GOR, and inverted triangles for 1.2 GOR.

Figure 11. Dynamic shear modulus of asphalt (G*).

Figure 11 shows that G* decreases with increasing temperature for all asphalts, indicating pronounced temperature susceptibility. Over the interval 34 °C–52 °C G* drops sharply with temperature; from 52 °C to 64 °C the rate of decrease moderates, and as the temperature rises further to 64 °C–82 °C the decline becomes progressively more gradual. At any given temperature, every GO dosage raises the G* of CRMA, increasing the elastic contribution and hence the resistance to deformation. The 0.3% GO blend exhibits the highest G*, demonstrating that a small GO addition effectively improves the high-temperature performance of CRMA. This improvement stems from the two-dimensional, high-specific-surface nano-lamellae of GO, which disperse uniformly throughout the asphalt and raise the overall stiffness of the asphalt. Through physical cross-linking, these sheets restrain the mobility of asphalt molecular chains, enhance the elastic response under dynamic shear loading, and thereby improve the modified asphalt’s resistance to load-induced deformation and stability at high temperatures.

3.3.2 Phase angle

The δ is the phase difference between deformation and applied stress in asphalt; it quantifies the viscous-versus-elastic contribution in such viscoelastic materials (Chen A. et al., 2021). When the δ of an asphalt increases, the viscous contribution dominates, so deformation produced under load is less recoverable; when the phase angle decreases, the elastic contribution grows, the material behaves more like an elastic solid, and it becomes less susceptible to high-temperature rutting. The δ of the modified asphalts are plotted in Figure 12.

Figure 12
Line graph showing the relationship between temperature (degrees Celsius) and phase angle (degrees) for various gas-oil ratios (GOR): CR, 0.3, 0.6, 0.9, and 1.2. Phase angle increases with temperature for all ratios. An inset details the 48 to 52 degrees Celsius range, highlighting slight variations between curves.

Figure 12. δ of GOR.

Figure 12 shows that the δ of all asphalt samples exhibits a rising trend with the rise of the temperature, indicating a growing viscous component within the material. This indicates that as temperature increase, the proportion of viscous components within the asphalt increases. From a macroscopic perspective, this means that the deformation experienced by the asphalt under load becomes more irreversible, diminishing its elastic recovery capability. When the GO dosage is 0.3%, the phase angle δ of GOR reaches its minimum, indicating that a low GO content reduces the proportion of CRMA that transforms into viscous components at elevated temperatures and thereby helps suppress the thermally-induced movement of asphalt molecules. This implies that the asphalt pavement is less likely to undergo permanent deformation when subjected to continuous, repeated vehicular loading in real-world applications.

3.3.3 Rutting factor

An index used to evaluate an asphalt’s resistance to permanent deformation is called the G*/sin δ; the higher the G*/sin δ, the stronger the rutting resistance and the bigger the deformation resistance (Camargo et al., 2022). The calculated rutting factors for the various asphalt blends are plotted in Figure 13. At any given temperature the GOR asphalts exhibit higher G*/sin δ than CRMA, the increase being most pronounced for the 0.3% GO blend. This demonstrates that a moderate GO dosage strengthened high-temperature rutting resistance of CRMA. The formation of a stable network structure, resulting from interactions between GO’s oxygen-containing functional groups and asphalt molecules, is the underlying mechanism for this improvement. This structure restricts the mobility of the asphalt molecules, which in turn enhances the overall stiffness and stability. However, stemming from its high specific surface area and surface energy, excessive GO tends to agglomerate; under high temperatures these agglomerates can act as stress-concentration sites and adversely affect both high-temperature stability and rutting resistance.

Figure 13
Graph showing the relationship between temperature (degrees Celsius) and rutting factor (Pascals) for five different materials: CR, 0.3GOR, 0.6GOR, 0.9GOR, and 1.2GOR. All exhibit a downward trend as temperature increases from 34 to 82 degrees Celsius. An inset highlights the range between 58 and 60 degrees Celsius, showing detailed variations among the material lines.

Figure 13. Rutting factor of GOR modified asphalt (G*/sin δ).

4 Conclusions and prospects

Targeting CRMA’s excessive viscosity and inadequate storage stability, this study developed GOR with superior overall performance. Different dosages of GO were incorporated into CRMA, and conventional property tests were used to assess the physical properties of the composite-modified asphalt. RTFOT and PAV were employed to simulate aging, and retained-penetration ratio together with softening-point increment were analyzed to assess aging resistance. Temperature sweep tests were then performed to obtain rheological parameters, thereby systematically revealing the improvement of CRMA high-temperature performance by GO. The principal findings are summarized as follows:

1. The introduction of an optimal amount of GO serves to enhance the high-temperature stability, low-temperature crack resistance, and storage stability of CRMA, thereby improving its overall performance.

2. Through interfacial reinforcement, GO effectively suppresses the evaporation of light fractions and the occurrence of oxidation reactions during asphalt aging, significantly improving the aging resistance of CRMA.

3. GO imparts improved high-temperature rheological performance of CRMA, as demonstrated by elevated G*/sin δ and G*, along with decreased δ, effectively enhancing the asphalt’s resistance to deformation and rutting.

4. Overall, utilizing CR can alleviate environmental pressures; although the unit price of GO is relatively high, its extremely low optimal dosage (0.3%) makes the cost increase manageable. The improvement in its comprehensive performance is expected to extend the service life of pavements, demonstrating good cost-effectiveness and sustainability from a life-cycle perspective.

5. Future work should elucidate the micro-scale interaction mechanism among GO, to encourage the widespread use of this material in green road building, CR and asphalt, rigorously assess the field performance of GOR combinations, and confirm their long-term service behavior through extensive demonstration projects.

Data availability statement

The original contributions presented in the study are included in the article/supplementary material, further inquiries can be directed to the corresponding author.

Author contributions

YW: Funding acquisition, Supervision, Methodology, Conceptualization, Investigation, Writing – review and editing, Data curation. YS: Data curation, Writing – review and editing, Formal Analysis, Methodology, Investigation. LH: Formal Analysis, Data curation, Project administration, Validation, Methodology, Writing – review and editing. XW: Conceptualization, Project administration, Visualization, Investigation, Writing – review and editing. CL: Methodology, Supervision, Conceptualization, Project administration, Writing – original draft, Investigation, Formal Analysis.

Funding

The author(s) declared that financial support was received for this work and/or its publication. The research is supported by the Guangxi Key Research and Development Program (Gui Ke AB23026067) and the Study on Road Performance of Green, Low-Carbon and Environmental-Friendly USP Asphalt in Complex Climates Scientific Research Topic (Project No.: 202302288), and this work received funding from China railway first group third engineering CO., LTD. The funder was not involved in the study design, collection, analysis, interpretation of data, the writing of this article or the decision to submit it for publication.

Conflict of interest

Authors YW, YS, LH, and XW were employed by China Railway First Group Third Engineering Co., Ltd.

The remaining author(s) declared that this work was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

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References

Cai, B., Ma, Y., Xiang, H., Zhong, J., Yuan, H., Zhang, Z., et al. (2025). Rheological characterization of high-content rubber modified asphalt considering particle size distribution. Case Stud. Constr. Mater. 22, e4594. doi:10.1016/j.cscm.2025.e04594

CrossRef Full Text | Google Scholar

Camargo, I., Hofko, B., and Mirwald, J. (2022). Effect of dltdp and furfural on asphalt binders: optimal dosage and pg grading. Constr. Build. Mater. 314 (125489A), 125489. doi:10.1016/j.conbuildmat.2021.125489

CrossRef Full Text | Google Scholar

Chen, A., Hu, Z., Li, M., Bai, T., Xie, G., Zhang, Y., et al. (2021). Investigation on the mechanism and performance of asphalt and its mixture regenerated by waste engine oil. Constr. Build. Mater. 313 (125411), 125411. doi:10.1016/j.conbuildmat.2021.125411

CrossRef Full Text | Google Scholar

Chen, M., Geng, J., Xia, C., He, L., and Liu, Z. (2021). A review of phase structure of sbs modified asphalt: affecting factors, analytical methods, phase models and improvements. Constr. Build. Mater. 294 (123610), 123610. doi:10.1016/j.conbuildmat.2021.123610

CrossRef Full Text | Google Scholar

Hou, X., Xiao, F., Wang, J., and Amirkhanian, S. (2018). Identification of asphalt aging characterization by spectrophotometry technique. Fuel 226, 230–239. doi:10.1016/j.fuel.2018.04.030

CrossRef Full Text | Google Scholar

Hoy, M., Suddeepong, A., Horpibulsuk, S., Akkharawongthattana, K., Arulrajah, A., Buritatum, A., et al. (2024). Improved performance of natural rubber latex-modified asphalt concretes with various types of aggregates. J. Mater. Civ. Eng. 36 (040234951), 04023495. doi:10.1061/JMCEE7.MTENG-16274

CrossRef Full Text | Google Scholar

Huang, J., Yan, K., Wang, M., Shi, K., Li, Y., and Zhang, Y. (2024). Performance evaluation of sbs-modified asphalt mixtures incorporating waste tire rubber and hdpe. Constr. Build. Mater. 430, 136423. doi:10.1016/j.conbuildmat.2024.136423

CrossRef Full Text | Google Scholar

Huang, W., Li, Y., Meng, Y., He, C., Ye, X., Chen, X., et al. (2024). Comprehensive study on the performance of sbs and crumb rubber composite modified asphalt based on the rubber pretreatment technology. Case Stud. Constr. Mater. 20 (e03141), e03141. doi:10.1016/j.cscm.2024.e03141

CrossRef Full Text | Google Scholar

Li, Y., Chai, J., Wang, R., Zhou, Y., and Tong, X. (2022). A review of the durability-related features of waste tyre rubber as a partial substitute for natural aggregate in concrete. BUILDINGS-BASEL 12, 197511. doi:10.3390/buildings12111975

CrossRef Full Text | Google Scholar

Li, T., Jiang, K., Liu, K., and Li, Q. (2025). Fourier transform infrared spectroscopy characterization of aging properties of graphene oxide modified asphalt binder. Int. J. Adhes. Adhes. 139 (103974), 103974. doi:10.1016/j.ijadhadh.2025.103974

CrossRef Full Text | Google Scholar

Li, H., Zhou, L., Cai, Y., Zhang, Y., Ibrahim, B. A., Feng, Z., et al. (2024). Potential applications for composite utilization of rubber and plastic in asphalt pavements: a critical review. J. Traffic Transp. Eng.-Engl. Ed. 11 (5), 939–971. doi:10.1016/j.jtte.2024.04.005

CrossRef Full Text | Google Scholar

Li, K., Yan, X., Wang, Y., Pu, J., Liu, W., and Jiang, S. (2024). Investigation of rheological properties and modification mechanism of sbs-modified asphalt with different warm mix additives. Int. J. Pavement Eng. 25 (23281301), 2328130. doi:10.1080/10298436.2024.2328130

CrossRef Full Text | Google Scholar

Li, L., Zhou, T., Cao, L., Zhou, J., Liu, Z., and Dong, Z. (2024). Characterization of emissions from rubber modified asphalt and their impact on environmental burden: insights into composition variability and hazard assessment. J. Hazard. Mater. 477, 135336. doi:10.1016/j.jhazmat.2024.135336

PubMed Abstract | CrossRef Full Text | Google Scholar

Liu, Z., and Gu, Q. (2025). Evolution of creep energy and damage constitutive model for waste tire rubber concrete. J. Build. Eng. 112, 113877. doi:10.1016/j.jobe.2025.113877

CrossRef Full Text | Google Scholar

Liu, L., Zong, J., Hou, X., and Liu, X. (2024). Effect of the inorganic modification mode on the mechanical properties of rubber recycled concrete. Materials 17, 221710. doi:10.3390/ma17102217

PubMed Abstract | CrossRef Full Text | Google Scholar

Peng, X., Pan, F., Lin, Z., Lv, S., and Liu, P. (2025). Experimental and molecular dynamics investigation of graphene oxide-modified bio-oil rejuvenated asphalt binder. Constr. Build. Mater. 494 (143354), 143354. doi:10.1016/j.conbuildmat.2025.143354

CrossRef Full Text | Google Scholar

Shatanawi, K. M., Biro, S., Geiger, A., and Amirkhanian, S. N. (2012). Effects of furfural activated crumb rubber on the properties of rubberized asphalt. Constr. Build. Mater. 28 (1), 96–103. doi:10.1016/j.conbuildmat.2011.08.041

CrossRef Full Text | Google Scholar

Su, J., Li, P., Zhu, G., Wang, X., and Dong, S. (2024). Interface interaction of waste rubber-asphalt system. BUILDINGS-BASEL 14 (18686), 1868. doi:10.3390/buildings14061868

CrossRef Full Text | Google Scholar

Tian, Y., Li, H., Zhang, H., Yang, B., Zuo, X., and Wang, H. (2021). Comparative investigation on three laboratory testing methods for short-term aging of asphalt binder. Constr. Build. Mater. 266 (121204B), 121204. doi:10.1016/j.conbuildmat.2020.121204

CrossRef Full Text | Google Scholar

Wen, Y., Liu, Q., Chen, L., Pei, J., Zhang, J., and Li, R. (2020). Review and comparison of methods to assess the storage stability of terminal blend rubberized asphalt binders. Constr. Build. Mater. 258 (119586), 119586. doi:10.1016/j.conbuildmat.2020.119586

CrossRef Full Text | Google Scholar

Yang, L., Zhou, D., and Kang, Y. (2020). Rheological properties of graphene modified asphalt binders, Nanomater. (Basel)., Rheological Properties Graphene Modified Asphalt Binders Nanomater. (10, pp. 2197) doi:10.3390/nano10112197

PubMed Abstract | CrossRef Full Text | Google Scholar

Yang, S., Zhu, H., Li, R., Yang, X., Tan, Q., Chen, Y., et al. (2024). Application of functionalized graphene oxide in the preparation of crumb rubber modified asphalt with excellent storage stability. Constr. Build. Mater. 450 (138488), 138488. doi:10.1016/j.conbuildmat.2024.138488

CrossRef Full Text | Google Scholar

Yu, H., Leng, Z., Zhang, Z., Li, D., and Zhang, J. (2020). Selective absorption of swelling rubber in hot and warm asphalt binder fractions. Constr. Build. Mater. 238 (117727), 117727. doi:10.1016/j.conbuildmat.2019.117727

CrossRef Full Text | Google Scholar

Zhang, X., Qiu, Y., Gao, Y., Zhao, X., Li, F., Huo, J., et al. (2024). Low-temperature performance of acrylonitrile-butadiene-styrene and crumb rubber compound-modified asphalt activated by waste cooking oil surface treatment. J. Mater. Civ. Eng. 36 (040242769), 04024276. doi:10.1061/JMCEE7.MTENG-18000

CrossRef Full Text | Google Scholar

Zhao, X., Li, F., Zhang, X., Qiu, Y., Lei, L., Zhao, Y., et al. (2024). Viscosity reduction mechanism and rheological properties of ethylene-bis-stearamide and crumb rubber modified asphalt. Constr. Build. Mater. 412 (134830), 134830. doi:10.1016/j.conbuildmat.2023.134830

CrossRef Full Text | Google Scholar

Zheng, W., Wang, H., Chen, Y., Ji, J., You, Z., and Zhang, Y. (2021). A review on compatibility between crumb rubber and asphalt binder. Constr. Build. Mater. 297 (123820), 123820. doi:10.1016/j.conbuildmat.2021.123820

CrossRef Full Text | Google Scholar

Keywords: aging resistance, conventional physical properties, crumb rubber modified asphalt, graphene oxide, high-temperature rheological properties

Citation: Wang Y, Sun Y, Huang L, Wang X and Lin C (2026) Study on the physical properties, anti-aging properties, and rheological characteristics of graphene oxide/rubber powder composite modified asphalt. Front. Mater. 12:1758696. doi: 10.3389/fmats.2025.1758696

Received: 02 December 2025; Accepted: 22 December 2025;
Published: 14 January 2026.

Edited by:

Chen Li, Inner Mongolia University, China

Reviewed by:

Linlin Zhu, Shandong Jianzhu University, China
Sun Keke, Shandong University, China

Copyright © 2026 Wang, Sun, Huang, Wang and Lin. This is an open-access article distributed under the terms of the Creative Commons Attribution License (CC BY). The use, distribution or reproduction in other forums is permitted, provided the original author(s) and the copyright owner(s) are credited and that the original publication in this journal is cited, in accordance with accepted academic practice. No use, distribution or reproduction is permitted which does not comply with these terms.

*Correspondence: Chanyuan Lin, MTAzMDYxNDA5M0BxcS5jb20=

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