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Nanotechnology Reviews

Editor-in-Chief: Hui, David

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Micro- structure and rheological properties of graphene oxide rubber asphalt

Mei Lin
• Corresponding author
• Research and Development Center of Transport Industry of Technologies, Materials and Equipments of Highway Construction and Maintenance (Gansu Road & Bridge Construction Group), Lanzhou 730030, Gansu, China
• School of Civil Engineering, Lanzhou University of Technology, Lanzhou Gansu, 730050, China
• Email
• Other articles by this author:
/ Zhao Li Wang
• Research and Development Center of Transport Industry of Technologies, Materials and Equipments of Highway Construction and Maintenance (Gansu Road & Bridge Construction Group), Lanzhou 730030, Gansu, China
• Other articles by this author:
/ Ping Wen Yang
• Research and Development Center of Transport Industry of Technologies, Materials and Equipments of Highway Construction and Maintenance (Gansu Road & Bridge Construction Group), Lanzhou 730030, Gansu, China
• Other articles by this author:
/ Ping Li
Published Online: 2019-11-12 | DOI: https://doi.org/10.1515/ntrev-2019-0021

Abstract

Compared with traditional materials, nanomaterial has rich and excellent performance due to the size advantages. If nanotechnology is combined with pavement materials, it is foreseeable that it will have a profound impact on the development of the road. In the study, graphene oxide nanomaterial was added as modifiers to rubber asphalt and its microstructure was characterized. The rheological properties of graphene oxide rubber asphalt and the road performance of asphalt mixture were studied in accordance with the SHRP test. The results showed that graphene oxide could form a dense and stable microstructure with rubber powder and asphalt polymer. As a modifier, it could improve the anti-rutting performance of rubber modified asphalt and was more suitable for heavy traffic. Moreover, it had low sensitivity to temperature and was more suitable for areas with large temperature difference between day and night. The pavement performance of the graphene oxide rubber asphalt mixture had also been greatly improved.

1 Introduction

Figure 1

The structure model of GO

Raw materials

The style of matrix asphalt was SK-90 (Whose penetration grade is 90#). 90 means the penetration of the asphalt binder at 25C ranging from 80 to 100 (units in 0.1 mm). The technical indicators were detected accordance with the “Standard Test Methods of Bitumen and Bituminous Mixtures for Highway Engineering” (JTG E20-2011), and the results were shown in Table 1. The indicators of matrix asphalt met the specification shown as in Table 1. The rubber powder was the A grade 40 mesh rubber powder. The technical specifications of grapheme was shown as in Table 2.

Table 1

Technical indicators of SK-90 asphalt

Table 2

Technical indicators of graphene oxide

Preparation method of rubberized asphalt

The three asphalt samples were prepared by melt blending method, mainly using high-speed shear emulsifier to disperse nano-material graphene, rubber powder and SBS modifier in asphalt.

2.2 Test methods

Graphene oxide rubber asphalt (GORA), rubber asphalt (RA) and SBS modified asphalt (SBSA) were selected as the research objects, and Scanning Electron Microscopy (SEM), multi-stress repeated creep (MSCR) and dynamic shear rheology (DSR) tests were performed. Mixing design of GORA, RA and SBSA asphalt mixture by rotary compaction with AC-13 as the mix structure type (calledAC-13-GR, AC-13-R,AC-13-SBS). High temperature stability, low temperature performance and water stability of the mixture were tested.

2.2.1 SEM test

The surface of three asphalt were observed by using a scanning electron microscopy (SEM, ZEISS, EVO18, Germany). The maximum magnification of SEM is 100,000 times. The specific methods for SEM test are followed: (1) Samples of three asphalt were melted into trichloroethylene to form the solution with a mass fraction of 10%. (2) The solution were uniformly dropped on a metal-like pile with a conductive cloth and dried under an infrared lamp. (3) The dry samples were sprayed as trichloroethylene was completely volatile. (4) SEM tests were carried out on samples.

2.2.2 DSR test

According to the SHRP plan, the three kinds of asphalt were subjected to DSR rheology test. The instrument used in the DSR test is a high precision TA-HR-1. The DSR test took the following two sweeping methods.

1. Temperature sweep (TS)

TS was in a stress-controlled loading mode with a test temperature range of 58C to 88C, an interval of 6C, a stress level of 100 Pa, and a test frequency of 10 rad/s.

2. Frequency sweep (FS)

FS was in strain -controlled loading mode with angular frequency range of 0.1~100 rad/s,which strain levelwas 1.25%. The three asphalt samples were subjected to FS test at 30C~70C.

2.2.3 Multi-stress creep recovery (MSCR)

MSCR was carried out for 10 times (Creep 1s, recovery 9s) at the temperature of 64C and shear stress of 0.1 kPa and 3.2 kPa using DSR tester.

2.2.4 High temperature stability test of mixture

Rutting test, which can be evaluated performance of rubber asphalt mixture at the high temperature ,were carried out on the asphalt mixtures in accordance with “Standard Test Methods of Bitumen and Bituminous Mixtures for Highway Engineering” (JTGE20-2011). The rutting plate samples with the size of 300 mm×300 mm×50 mm were formed according to rolling method at the temperature of 60C and pressure of 0.7 MPa.

2.2.5 Low temperature performance test of mixture

The bending test of the trabecular, which could evaluate the performance of the rubber asphalt mixture at low temperature, were performed on the asphalt mixtures with two grades and three contents according to JTG E20-2011. The trabecular specimens were formed with rock cutting machine. Firstly, rutting plate samples were cut into beam specimens with the size of 250mm×30mm×35mm. Secondly, the trabecular specimen was in incubator at −10C for 3 hours before test. Lastly, the bending test of the trabecular was carried out at the temperature of −10C and a loading rate of 50mm/min.

2.2.6 Water stability test of mixture

The cylindrical marshall specimens with size of 101.6×63.5mm after repeated freeze-thaw cycles was tested by the Marshall Stability meter produced by Changsha Yaxing Company. Specimens of repeated freeze-thaw cy cles were tested as follows: (1) The specimens were been for 15 min under a vacuum of 98.0 KPa. (2) Normal pressure was restored, and the specimens keep for 0.5h in the sink of constant 25C. (3) The test pieces were placed in a plastic bag containing 10 ml of water and frozen for 6h in a refrigerator with constant temperature of −20C. (4) The specimen was placed in a sink with constant temperature of 25C and melt for 2 hours. The four steps were a freeze-thaw cycle. The split test was carried out according to the conditions of the freeze-thaw cycle for 0, 3, 6, 9 and 12 times.

3.1 Testing of three asphalt samples

The three asphalt samples of GORA, RA, SBSA were tested. The test results were provided in Table 3.

Table 3

Technical indicators of asphalt samples

As given in Table 3, general performance indicators of GO had been improved compared to RA and SBSA.

3.2 Microstructure analysis of materials

The microstructures of GO, RA, GORA, SBSA scanned scanned by SEM were shown in Figure 3.

Figure 2

Microstructure of asphalt samples

Figure 3

The complex modulus master curve of 40C

Figure 2(a) showed that rich oxygen-containing groups were attached to the base surface and the edge of the graphene Oxide structural unit, and these oxygen-containing groups mainly included -COOH, -OH, C=0, and epoxy-0-. These oxygen-containing groups provide a large number of active sites for the functionalization of the surface of GO. Figure 2(b) showed that the rubber particles with irregular shape could not be dissolved in the asphalt, which were wrapped by binder. There was a good adhesion between particles and binder for two-phase interface united closely. Figure 3(c) illustrated the addition of GO to rubber asphalt to form a denser and more stable grid structure. Figure 3(d) showed SBS modified asphalt had agglomerated.

3.3 Rheological parameter analysis

According to SHRP, the shear frequency can be correlated with the amount of road traffic. When the shear frequency is between 0.01 and 100 Hz, it can simulate the normal traffic on the road. Higher frequencies simulate heavier traffic, whereas lower frequencies simulate lighter traffic [40, 41]. Therefore, when the shear frequency is 10−3 to 103 Hz, it can represent the entire traffic condition. According to the time-temperature equivalent principle [42, 45], the main curve in the wide frequency range of 40C was synthesized by horizontal displacement superposition, and the relationship between the frequency and the composite modulus G* was obtained, as shown in Figure 3.

It could be seen from Figure 3 that the composite modulus G* of the three kinds of asphalt decreased with the decrease of temperature. The modulus value of GORA was the highest under the same temperature, which indicated that the viscoelasticity of GORA increased with the increase of traffic volume, and the sensitivity of change was lower than that of the other two modified asphalts. Therefore, GORA was more suitable for heavy traffic and large temperature difference between day and night.

The rutting factor is used to evaluate the ability to resist permanent deformation at high temperatures. The curve of rutting factor with temperature was shown as Figure 4.

Figure 4

Relationship between G*/ sin δ and T

It could be concluded from Figure 4 that GORA had the best rutting resistance, followed by RA and SBSA. This is due to the fact that GORA’s denser and more stable microscopic internal structure increases its ability to resist external loads.

The phase angle reflects the ratio of the elastic component to the viscous component in the test samples. The curve of phase angle with temperature was shown as Figure 5.

Figure 5

Relationship between δ and T

From Figure 5, the phase angle of GORA did not change significantly with temperature, and was basically maintained at about 50,which indicated that the viscoelasticity of GORA has little effect on temperature. SBSA showed more flexibility. The phase angle of RA showed an increasing trend with temperature, which indicated that RA was more sensitive to temperature than the other two types of asphalt. This result also showed that GORA was more suitable for the climate with large temperature difference between day and night.

3.4 Results of MSCR

According to the strain collected by the test, Jnr and Jnrdiff (Jnr-dependent change rate of stress) under different stresses were calculated. The calculation method was as Table 4:

Table 4

The MSCR results of GORA

$Jnr=εr−ε0δ$(1)$Jnr−diff=Jnr(3.2k Pa)−Jnr(0.1k Pa)Jnr(3.2kPa)$(2)

ε0 – Initial deformation; εr – Residual deformation after 9s recovery; δ – Shear stress

It could be seen from Table 4 that the Jnr−3.2 of GORA and RA at 64C was 0.15 times and 0.26 times of SBSA, and both were less than 0.5, which is a heavy load standard. The Jnr-diff of GORA was 0.17 and 0.10 smaller than RA and SBSA, respectively, which indicated that GORA was less sensitive to the increase of stress level than RA/SBSA. So, it indicated that GORA was more suitable for heavy traffic.

3.5 High temperature rutting test of mixture

The rutting test of AC-13 were carried out in the study. In order to reduce the test error, three parallel tests were carried out for each sample, and the average values were obtained. The Dynamic stability of AC-13 were shown in Table 5.

Table 5

Dynamic stability of GORA mixture

The dynamic stability (DS) of the GORA mixture was significantly more improved than that of the other two mixture. The test result investigated that anti-rutting performance was GORA > SBSA > RA.

3.6 Low temperature trabecular test of mixture

The test on beam bending at low temperature was performed for AC-13, and the results were shown in Table 6.

Table 6

Low temperature cracking test of GORA mixture

3.7 Water stability test of mixture

The Marshall test was carried out to evaluate water stability. The results of the Marshall test on AC-13–GR , AC-13-RA and AC-13-SBS were presented in Table 7.

Table 7

Water stability test of GORA mixture

The experimental results indicate that the addition of GO could significantly improve the durability of asphalt mixture.

4 Conclusion

A rich oxygen-containing group is attached to the base surface and the edge of the GO structural unit. These oxygen-containing groups provide a large number of active sites for the functionalization of the surface of GO. Therefore, mixing GO with rubber powder and asphalt polymer can form a more dense and stable structure.

Through rheological tests, it is found that GORA has better high-temperature rutting resistance and lower temperature sensitivity than RA and SBSA, and is more suitable for heavy traffic and large temperature difference between day and night.

Through the rutting test, low temperature bending test and freeze-thaw splitting test of the asphalt mixture, it was found that the GORA mixture achieved good road performance.

Acknowledgement

This work was supported by the Research and Development Center of Transport Industry of Technologies, Materials and Equipments of Highway Construction and Maintenance (Gansu Road & Bridge Construction Group) Open Fund (No. GLKF201814), the National Natural Science Foundation of China (Nos. 51868047, 51668041), the Fundamental Research Funds for the Central Universities (31920180077).

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Accepted: 2019-06-07

Published Online: 2019-11-12

Citation Information: Nanotechnology Reviews, Volume 8, Issue 1, Pages 227–235, ISSN (Online) 2191-9097,

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