Laboratory Investigation of

Biochar-Modified Asphalt Mixture

Sheng Zhao, Baoshan Huang, Xiang Shu, and Philip Ye

The United States is promoting the establishment of a bio-based mesolength carbon fibers show high resistance to permanent defor-
economy, generating energy and fuels from renewable organic mat- mation, high tensile strength at low temperatures (7 ), and high
ters rather than fossil fuels. Byproducts such as fractions of biochar fatigue resistance (8). However, addition of mesofibers might pro-
not suitable for biofuel production are drawing extensive attention. duce fiber clumps, thus leading to poor dispersion of fibers and
(“Biochar” is defined by Oxford’s online dictionary as “charcoal pro- nonuniform mixing (7, 9). This result would limit the application
duced from plant matter and stored in the soil as a means of removing of mesofibers in asphalt industry. With the emergence of nano-
carbon dioxide from the atmosphere.”) Recently, biochar produced technology in the last decade or so, nanosized carbon fibers were
with different production parameters was tried as an asphalt modi- used by highway engineers in pavement engineering (10, 11). The
fier owing to its carbon origin and proved to be positive in binder nanocarbon fibers behave more like nanoparticles rather than act-
modification. This study evaluated the performance of hot-mix asphalt ing as fiber owing to the extremely small size, although a uniform
modified by one type of pyrolytic biochar with controlled production mixing can be achieved.
parameters. Typical carbon black powder pellets and microsized carbon Carbon black has been known to have a dramatic reinforcing
fiber were selected as the reference additives. Multiple laboratory binder effect on rubbers, showing potential benefits as an additive to asphalt
and performance tests were conducted to evaluate the rheological prop- binder owing to its carbon origin (12). Extensive research has shown
erties of the modified binder, rutting resistance, moisture susceptibility, that pelletized carbon black can reduce the temperature susceptibility
and cracking resistance of asphalt mixtures. On the basis of test results, of asphalt (12–14), improve rutting resistance at high temperatures
the biochar evaluated in this study proved to be an effective modifier in (14–16), and reduce stripping potential (16) while maintaining simi-
reducing the temperature susceptibility of the binder and thus increased lar fatigue and tensile characteristics of the mixtures (15, 16). The
the rutting, moisture, and cracking resistance of hot-mix asphalt. In previous studies acknowledged the usefulness of carbon black as a
addition, biochar proved to be a better asphalt modifier than did carbon reinforcing agent; however, the fatigue and cracking resistance of the
black and carbon fiber. asphalt mixtures modified by carbon black may remain a significant
concern.
During recent years, the United States has been promoting the
Carbonaceous materials have long been used as asphalt additives bio-based economy by requiring that energy and fuels be gener-
because they are made of carbon and considered to be inherently ated from renewable organic matters rather than fossil fuels (17).
compatible with asphalt binder that is hydrocarbon (1). This Some byproducts, which are not suitable for biofuel production
expectation has motivated numerous studies since the 1960s (2) to and not used in any other industry, are drawing extensive atten-
modify asphalt binder with carbon-based materials for improved tion. Fractions of biochar are one such byproduct from pyrolysis
performance. Among the many carbonaceous materials, carbon of biomass. (“Biochar” is defined by Oxford’s online dictionary as
fiber and carbon black are commonly selected by researchers as “charcoal produced from plant matter and stored in the soil as a
asphalt additives owing to their easy availability. means of removing carbon dioxide from the atmosphere.”) Most
The majority of carbon fiber research in the construction indus- previous studies on biochar have been focused on its capability as
try has been on its addition to concrete mixes (3, 4). The intro- a soil amendment that improves the physical and chemical prop-
duction of carbon fiber into asphalt stems from the hope that its erties of soil and may enhance nutrient cycling and plant growth
high tensile strength may possibly increase the cracking resistance (18, 19). Since aforementioned carbon-based modifiers have been
of asphalt pavement (1). It is also found that addition of carbon successfully applied in asphalt modification, it is highly likely that
fibers produces electrically conductive asphalt mixtures (5, 6). biochar can be used as a biomodifier in asphalt mixture to improve
Previous studies have shown that asphalt mixtures modified with the performance of asphalt mixtures. Earlier research work (20)
evaluated asphalt binder modified with biochar prepared with dif-
ferent production parameters, demonstrating that biochar reduced
S. Zhao, B. Huang, and X. Shu, Department of Civil and Environmental Engineering, the temperature susceptibility and long-term oxidation of asphalt
University of Tennessee, Knoxville, 851 Neyland Drive, Knoxville, TN 37996-2323.
P. Ye, Department of Biosystems Engineering and Soil Science, University of
binders, significantly increased the rutting resistance at high tem-
Tennessee, Knoxville, 2506 E. J. Chapman Drive, Knoxville, TN 37996-4531. peratures, and showed little or slightly better fatigue resistance. It
Corresponding author: B. Huang, bhuang@[Link]. was also found that the most effective biochar was the one with
small particle size and that produced at a comparably lower treat-
Transportation Research Record: Journal of the Transportation Research Board,
No. 2445, Transportation Research Board of the National Academies, Washington,
ment temperature and heating rate. However, performance of the
D.C., 2014, pp. 56–63. asphalt mixtures with biochar-modified binder is still unknown and
DOI: 10.3141/2445-07 needs to be further investigated.

56
Zhao, Huang, Shu, and Ye 57

TABLE 1   Asphalt Mixtures Evaluated in the Study

Asphalt Mixture Additive Additive Content (%)

PG 64-22 control mix na na

Modified mix Biochar 5
10
Carbon black 5
10
Carbon fiber 5
10

Note: na = not applicable.

Objective and Scope FIGURE 1   Direct view of additives.

The objective of the study is to evaluate the laboratory performance

of hot-mix asphalt (HMA) produced with binders modified with
selected biochar. The biochar used in this study was the most effec- Laboratory Experiments
tive one selected from the previous research (20). Microsized carbon
fibers and carbon black powder pellets were selected as reference Materials
additives based on previous discussion. Rheological properties of
the modified binder, rutting resistance, moisture susceptibility, and The biochar used in this study was produced with a tube-furnace
cracking performance of the mixture were tested. pyrolysis method (slow pyrolysis) based on a previous study (20).
Six modified mixtures with various additive contents up to 10% Production parameters are as follows:
by weight of the asphalt and one control mixture with virgin binder
only were evaluated in this study (Table 1). The maximum additive • Starting temperature = 25°C,
content of 10% was determined on the basis of previous binder– • Pyrolysis temperature = 400°C,
mastic investigation (20) and studies on other carbon-based modi- • Heating rate = 15°C/min,
fiers (13, 16, 21). The complex shear modulus (G*) obtained from • Pyrolysis duration = 60 min, and
the dynamic shear rheometer (DSR) test was used to show the effect • Biochar production rate = 27.92%.
of additives on rheological properties of asphalt binder–mastic. The
resilient modulus (MR) and asphalt pavement analyzer (APA) rutting Only the particles smaller than 75 µm were used in this study to
tests were employed to characterize rutting resistance of the modi- achieve homogeneous and uniform mixing. Switchgrass was used
fied mixture, while the AASHTO T 283 test after a freeze–thaw as the biomass source since considerable effort is presently being
cycle was conducted to evaluate the moisture susceptibility pertain- expended to make switchgrass a potential biofuel source (28). A
ing to tensile strength ratio (TSR) and MR ratio. The dissipated creep commercially available carbon black with an average diameter of
strain energy (DCSEf) (22) from the Superpave® indirect tension 80 nanometers (nm) and surface area of more than 20 m2/g was
(IDT) tests and the J-integral from the semicircular bending (SCB) used in this study. The carbon fiber was approximately 6 to 7 µm in
notched fracture test (23–27) were used to evaluate the cracking diameter, and tensile strength and modulus of elasticity were 4,200
performance. to 4,550 MPa and 230 GPa, respectively. Figures 1 and 2 show

FIGURE 2   Images of additives magnified by SEM.

58 Transportation Research Record 2445

TABLE 2   Properties of Aggregates No. 10 screening, and 25% natural sand, and they met the grada-
tion specifications of the Tennessee Department of Transportation
Sieve Size Gravel No. 10 Natural (Figure 3). The optimum asphalt content was determined for control
(mm) D-Rock (%) Screening (%) Sand (%)
mix at 5.7% by weight of the total mix. To evaluate the effects of
16 100 100 100 the modified binders, 5.7% virgin asphalt–modified asphalt was held
constant for all the mixtures.
12.5 92 100 100
9.5 71 100 100
4.75 23 93 98
Sample Preparation
2.36 15 59 76
0.60 9 22 37 Asphalt binders and aggregates were heated for 2 h in an oven at
0.30 6 15 17 165°C before mixing. Meanwhile, the carbon-based additives were
0.15 4.0 11.4 7.0 dried at 120°C for 2 h and then blended with heated asphalt binders
0.075 2.5 9.5 3.2 at target concentrations by use of a mixing device designed for mas-
tic research (29) in the laboratory. Samples for the DSR test were col-
Note: Gsb (bulk specific gravity) = 2.511 for gravel D-rock; 2.704 lected immediately after the blending, and then the modified binders
for No. 10 screening; and 2.498 for natural sand. were mixed in the laboratory with heated aggregates for 2 min. The
newly produced mixtures were then kept in the oven for 2 h for short-
term aging before compaction. Cylindrical samples 150 mm high by
the ordinary picture and the scanning electron microscope (SEM) 100 mm in diameter were compacted with the Superpave gyratory
images of the different additives. Figure 1 shows that all three addi- compactor. The virgin binder for control mix was stirred for the same
tives appeared to be similar black powder. However, SEM images period of time before compaction to minimize the variations caused
show very different structures and surface textures. Carbon black by mixture production. The air voids of samples for the IDT tests and
was made of microcarbon pellets with a smooth texture, while car- SCB notch test were 4% ± 0.5%, and those for the APA and TSR tests
bon fiber was of a rod-like geometry and very fibrous nature. Bio- were 7% ± 1% so as to simulate volumetric properties of pavement
char comprised irregularly shaped particles with a porous structure, after several years’ service and at early service stage, respectively.
which may behave like a combination of porous carbon fiber and
micro­particles. In addition, its porous and rough surface textures may
help the interaction between biochar and asphalt binder, leading to Binder and Mixture Performance Testing
improved performance of asphalt mixture.
One commonly used asphalt binder in Tennessee with PG 64-22 DSR Test
was used to make all the mixtures. The coarse aggregate was gravel
D-rock with a nominal maximum aggregate size of 9.5 mm. The The effects of different types of biochar on binder modification were
fine aggregates consisted of No. 10 (2 mm) screenings and natural investigated in a previous study (20). In this study, the DSR test was
sand. Their gradations and other properties are presented in Table 2. conducted just to show the different properties of virgin and modi-
fied asphalt binders caused by additive modification. The complex
shear modulus (G*) of the virgin and modified binders was obtained
Mix Design from the DSR test by using samples of 8 mm diameter according
to AASHTO T 315. Since a PG 64-22 binder was used, 64°C and
The Marshall mix design procedure was employed to design the −10°C were selected to characterize the modification at high and low
mixtures. The aggregates consisted of 50% gravel D-rock, 25% service temperatures at a loading frequency of 10 rad/s.

100

90

80

70
Percentage Passing

60

50

40 Aggregate
Gradation
30
Lower Limit
20
Upper Limit
10

0
0.1 1 10
Sieve Size (in.)

FIGURE 3   Aggregate gradation and Tennessee Department of Transportation gradation limits.
Zhao, Huang, Shu, and Ye 59

Resilient Modulus Test σ

The MR (resilient modulus) test was part of the Superpave IDT tests
St
developed by Roque and Buttlar (30, 31). The test was conducted
at 25°C with procedures addressed elsewhere (32, 33). The MR for
each mixture was calculated with the following equation:

MR
P × GL
MR = (1) DCSEf EE
∆H × t × D × Ccmpl
ε0 εf ε
where
FIGURE 4   Calculation of DCSE f (34).
MR = resilient modulus (psi),
P= maximum load (lbf),
GL = gauge length (in.), A higher DCSEf value generally indicates a capability of accom-
ΔH = horizontal deformation (in.), modating more dissipated energy in the mixture, thus leading to
t= thickness of sample (in.), a better fatigue resistance of asphalt mixtures. Figure 4 presents
D= diameter of sample (in.), a schematic diagram for calculating DCSEf, where εf is the failure
Ccmpl = nondimensional creep compliance factor, strain, MR is the resilient modulus, EE is elastic energy, and St is
0.6354(X/Y)−1 − 0.332, and indirect tensile strength.
(X/Y) = ratio of horizontal to vertical deformation.

Semicircular Bending Notched Fracture Test

Asphalt Pavement Analyzer Rutting Test
The SCB fracture test was conducted on specimens with different
The APA rutting test was performed at 64°C in accordance with notch depths at 25°C at a constant rate of 0.5 mm/min. The critical
AASHTO T 340. Rut depths at 8,000 cycles were recorded for value of the J-integral was obtained and used as an indicator of
evaluating rutting resistance of the mixtures. fracture resistance of asphalt mixtures (23, 27). Three notch depths
were used in this study: 7.6 mm (0.3 in.), 15.2 mm (0.6 in.), and
25.4 mm (1 in.). The strain energy to failure was calculated for each
MR Ratio and TSR Tests notch as the numerical number of the area under the load versus
vertical deflection curve up to the peak load. Then the following
Both the MR ratio and TSR tests were used to determine the mois- equation was used to determine the critical J-integral:
ture susceptibility of asphalt mixtures by calculating the ratio of

()
MR and tensile strength of unconditioned to conditioned samples
1 dU
with 7% ± 0.5% air voids at 25°C (34). AASHTO T 283 was Jc = − (2)
followed for the indirect tensile strength (ITS) and freeze–thaw b da
conditioning procedures. A TSR value of 0.8 is recommended in
AASHTO M 320 as a criterion for good resistance to moisture where
susceptibility.
Jc = J-integral (kJ/m2),
b = thickness of specimen (m),
a = notch depth (m), and
Dissipated Creep Strain Energy Threshold U = strain energy to failure (kJ).
The DCSEf was obtained from the Superpave IDT tests (30, 31) and All the samples evaluated in this study were made in triplicate.
used to evaluate the cracking resistance of asphalt mixtures (35). The summarized experimental matrix is presented in Table 3.

TABLE 3   Experimental Matrix

Property Temperature Samples per

Evaluated Test (°C) Parameter Mixture

Rheology DSR 64 Ga 3
DSR −10 Ga 3
Rutting Superpave IDT 25 MR 3
resistance APA 64 Rut depth 3
Moisture Superpave IDT 25 MR ratio 3a
susceptibility TSR 25 TSR 3a
Cracking Superpave IDT 25 DCSEf 3
performance SCB 25 Jc 3
a
For MR ratio and TSR tests, triplicates were made for both conditioned and unconditioned
samples.
60 Transportation Research Record 2445

Results and Discussion 6,000

Resilient Modulus (MR)

5,000
Rheological Properties of Modified Binders
4,000
Figures 5 and 6 show the G* results at high and low temperatures,

(Mpa)
respectively. The observation that G* increased with the addition of 3,000 5%
the additives is as expected. It seems that biochar showed the high- 2,000 10%
est stiffening effect at high service temperatures, and that may lead
to a higher rutting resistance of the modified binder, but the differ- 1,000
ences in stiffening caused by the three carbonaceous additives were 0
not significant. For low temperatures, it can be seen in Figure 6 that Control Biochar Carbon Carbon
biochar showed very little effect on G* at −10°C, consistent with Mix Black Fiber
the findings from the previous study (20). However, the addition
of both carbon black and carbon fiber significantly increased the FIGURE 7   M R results at 258C.
G* of the binder at low temperatures, thus potentially leading to
a poor resistance of asphalt mixture to low temperature cracking. 10
This observation indicates that biochar was a more effective asphalt

APA Rut Depth (mm)

modifier, compared with carbon black and carbon fiber, for reducing 8
the temperature susceptibility of asphalt binder.
6
5%
4
Rutting Resistance 10%
2
The MR can be used as an indirect indicator of the rutting resis-
tance of asphalt mixtures. The higher the MR value, the higher the 0
rutting resistance of an asphalt mixture. Figure 7 illustrates the Control Biochar Carbon Carbon
MR results for the mixtures. It is observed that all three additives Mix Black Fiber
increased the MR if added up to 10%. This result can be attributed
to the stiffening effect of the solid powder-like additives. The fact FIGURE 8   APA rut depth results.
that carbon fiber showed an insignificant effect can be related to
its interaction with the binder. The rod-like microfibers may not
be uniformly blended with the binder-aggregate matrix during the
mixture production, thus resulting in a slightly poor structure of the
4.5E+3 matrix, although the carbon fibers were cut into microsizes. It was
found that the 10% biochar-modified mixture showed the highest
Complex Shear Modulus

4.0E+3
3.5E+3 MR, an indication that biochar may have a better interaction with
(G*) 64°C (Pa)

3.0E+3 the binder during mixing, and that may lead to a better resistance to
2.5E+3 rutting distress.
2.0E+3 5% Figure 8 presents the rut depths after 8,000 cycles from the APA
1.5E+3 rutting test. It is evident that the addition of the additives improved
10%
1.0E+3 the rutting resistance, especially biochar and carbon black at higher
5.0E+2 contents. This observation was consistent with results from the G*
0.0E+0 at high service temperature and MR. It is expected that carbon black
Control Biochar Carbon Carbon and carbon fiber could reduce the rut depths, especially carbon black
Binder Black Fiber (16). However, it was found that biochar showed a similar capability
of improving rutting resistance and thus was very promising as an
FIGURE 5   G* results at high service temperature (648C). additive in reducing rut distress.

4.0E+8
Complex Shear Modulus

3.5E+8 Moisture Susceptibility

3.0E+8
(G*) –10°C (Pa)

Figures 9 through 12 present the MR ratio, dry ITS, wet ITS, and
2.5E+8
TSR results, respectively. Generally, moisture resistance was slightly
2.0E+8 5% increased in most mixtures. The 10% addition of carbon black
1.5E+8 appeared to result in an obvious decrease in modulus but dem­onstrated
10%
1.0E+8 that it could satisfy the AASHTO specification of TSR being over 0.8.
5.0E+7 The modifier content was found to affect moisture resistance with the
0.0E+0 following tendency: the more modifiers that were added, the more
Control Biochar Carbon Carbon susceptible the mixture became to moisture. The mixtures modified
Binder Black Fiber with 10% carbon black or carbon fiber were found to be on the verge
of meeting the 80% TSR criterion, while the biochar-modified mix-
FIGURE 6   G* results at low service temperature (2108C). tures could easily meet this requirement, an indication that biochar
Zhao, Huang, Shu, and Ye 61

may have a higher capability of improving moisture resistance than

0.9 the other two carbon-based additives.
0.8
0.7
0.6 Cracking Performance
MR Rao

0.5
0.4 5% The DCSEf value has been successfully used to evaluate the cracking
0.3 resistance of asphalt mixtures (35, 36). The results are presented in
10%
0.2 Figure 13. It can be seen that high variations were observed in this
0.1 study, consistent with previous research using the same method (36).
0 So the numerical average of the triplicate was selected to conduct the
Control Biochar Carbon Carbon data analysis. Unlike the effects of the additives on other properties,
Mix Black Fiber the effects of the three additives were found to be noticeably differ-
ent from each other in regard to cracking resistance. The increase in
FIGURE 9   M R ratio results. the biochar or carbon black content reduced the DSCEf value, there-
fore compromising the cracking resistance of modified mixtures.
1.2 However, the 5% biochar was found to increase the DCSEf value,
1 and even the mixture with 10% biochar showed a similar DCSEf
result compared with the control mix. Meanwhile, carbon black
Dry ITS (Mpa)

0.8 did not show beneficial effect on cracking resistance, even added
0.6 in a small amount (5%). Carbon fiber behaved differently with the
5% increase in its content. Its modification effect was insignificant when
0.4 10% added at 5%. However, its effect became significant at a dosage of
0.2 10%. This phenomenon can be attributed to the fibrous nature
of the carbon fiber. It may function like reinforcement in concrete,
0 bridging the cracks and arresting crack propagation, thus leading to
Control Biochar Carbon Carbon a higher cracking resistance. The carbon fiber may perform even
Mix Black Fiber better at higher contents. However, use of this fibrous material may
FIGURE 10   ITS for unconditioned (dry) samples. be limited by such concerns as workability, dispersion, and moisture
susceptibility.
The J-integral concept has been successfully used to character-
1
ize the fracture resistance of the asphalt mixtures (23). Figures 14
and 15 show the change of the dissipated strain energy with the
0.8
notch depth. The J-integral was obtained for each mix accordingly
Wet ITS (Mpa)

0.6 and was reported in Figure 16. Samples with a 7.6-mm notch in
10% carbon black group were broken during the production, so the
5% Jc value for that mixture was obtained on the basis of two points.
0.4
10% As can be seen in Figure 16, the effects of additives in regard to the
0.2 J-integral were similar to that obtained from DCSEf results. Biochar
increased the Jc value so as to increase the cracking resistance of
0 the mixture. Carbon black showed adverse effects on the mixture in
Control Biochar Carbon Carbon regard to Jc value results, while carbon fiber proved to be positive
Mix Black Fiber when added in a higher amount. This consistency validates the con-
clusions drawn from Superpave IDT results and further indicates
FIGURE 11   ITS for conditioned (wet) samples. the effectiveness of biochar as an asphalt modifier.

1
10
0.8
8
0.6
DCSEf (kJ/m3)
TSR

5% 6
0.4
10% 5%
4
0.2 10%
2
0
Control Biochar Carbon Carbon 0
Mix Black Fiber Control Biochar Carbon Carbon
Mix Black Fiber
FIGURE 12   TSR results.
FIGURE 13  DCSE f results.
62 Transportation Research Record 2445

60 evaluated as reference materials. According to the test results,

conclusions can be summarized as follows:
50
Strain Energy (J/m)

1. Compared with carbon black and carbon fiber, biochar was

40 more capable of reducing the temperature susceptibility of the
Control Mix asphalt binder.
30
5% Biochar
2. MR and APA rutting test results indicated that biochar increased
the rutting resistance of the asphalt mixture.
20 5% Carbon Black 3. Biochar performed in a way similar to carbon black in
10 5% Carbon Fiber improving rutting resistance and did better than carbon fiber.
4. Biochar could reduce the moisture susceptibility of HMA
Linear (Control Mix) with addition of small amounts. The modification effect would be
0
0 10 20 30 compromised with the increase of the additive content.
Notch Depth (mm) 5. Biochar performed better than carbon black and carbon fiber
in improving the moisture resistance of HMA.
FIGURE 14   Change of strain energy with notch depth 6. Both DCSEf results from Superpave IDT tests and J-integral
(5% additive).
results from the SCB notched fracture test suggested that biochar
might increase the cracking resistance of HMA.
60 7. Carbon black might adversely affect the cracking resistance of
HMA, while carbon fiber might have a positive effect if added to a
50 certain amount. With the increase of additive content, the modifica-
tion from biochar might be compromised, whereas that of carbon
Strain Energy (J/m)

40 Control Mix
fiber was positively improved.
10% Biochar 8. Results presented in this paper were only the preliminary find-
30 ings of a more complete study. Further studies would be needed
10% Carbon Black
before biochar can be widely used in pavement engineering.
20 10% Carbon Fiber

Linear (Control Mix)

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