Effect of Morphology on High- Temperature Rheological …/12... · • A quantitative morphological...

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Workshop Swedish Node in Nordic Research School for Pavement Engineering Jiqing Zhu Swedish National Road and Transport Research Institute (VTI) [email protected] Effect of Morphology on High- Temperature Rheological Properties of Polymer-Modified Bitumen September 24 – 25, 2018, Hotel C, Stockholm

Transcript of Effect of Morphology on High- Temperature Rheological …/12... · • A quantitative morphological...

Page 1: Effect of Morphology on High- Temperature Rheological …/12... · • A quantitative morphological parameter for PMB, i.e. the characteristic wavelength ξ by 2D-FFT method. •

Workshop Swedish Node in Nordic Research School for Pavement Engineering

Jiqing Zhu Swedish National Road and Transport Research Institute (VTI)

[email protected]

Effect of Morphology on High-

Temperature Rheological Properties of Polymer-Modified Bitumen

September 24 – 25, 2018, Hotel C, Stockholm

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•  Background

•  Materials and Method

•  Results and Discussion

•  Summary

Contents

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Background

Material property

Composition

Structure

Processing

•  Polymer-modified bitumen (PMB) - Styrene-butadiene-styrene (SBS) copolymer •  Studies on PMB morphology-rheology relationship - Mostly used additives: e.g. sulfur, carbon nanotubes - Another angle?

HOT!

SBS modification

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Property   Base bitumen   Polymer-modified bitumen  

Penetration, 25 °C (0.1 mm)   86   56  

Softening point, ring & ball (°C)   43.4   77.8  

Penetration index   -1.8   4.3  

Materials •  Base bitumen 70/100 Pen. - 8% of saturates, 55% of aromatics, 22% of resins, 15% of asphaltenes •  Linear triblock SBS copolymer •  Polymer content: 5% by weight

of the blend PMB

Bitumen

Bitumen SBS

Materials and Method

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Materials and Method

•  Isothermal annealing of PMB - 2 samples: conditioned at 160 °C & 120 °C for 1h respectively

•  Microscopy observation and image analysis - Fluorescence microscopy - 2D fast Fourier transform (2D-FFT)

•  Rheological characterization (high-temperature) - Dynamic Shear Rheometer (DSR) - ASTM D7175: Complex modulus (G*) & phase angle (δ) @ (64 °C, 70 °C, 76 °C, 82 °C) × (10 rad/s, 1 rad/s, 0.1 rad/s) - ASTM D7405: Multiple stress creep and recovery (MSCR) @ 76 °C, 70 °C and 64 °C - Linear viscoelastic region & Low shear viscosity

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Results and Discussion - Morphology

2D-FFT

•  Power spectrum of imgae 𝑓(𝑟↓1 , 𝑟↓2 )

•  𝐹(𝑘↓1 , 𝑘↓2 ) is the Fourier transform. Its discrete form:

•  Characteristic wavelength 𝜉= 2𝜋/𝑘↓𝑚  

•  𝑘↓𝑚  is the characteristic spatial frequency (peak).

𝑃(𝑘↓1 , 𝑘↓2 )= |𝐹(𝑘↓1 , 𝑘↓2 )|↑2 

𝐹(𝑘↓1 , 𝑘↓2 )= 1/𝑁 ∑𝑟↓1 =0↑𝑁−1▒∑𝑟↓2 =0↑𝑁−1▒𝑓( 𝑟↓1 , 𝑟↓2 ) 𝑒↑−𝑗2𝜋/𝑁 ( 𝑘↓1 𝑟↓1 + 𝑘↓2 𝑟↓2 )   

𝑘=√𝑘↓1 ↑2 + 𝑘↓2 ↑2  

𝜉 = 0 mm = 0 mm

𝜉 = 2.356 mm = 2.356 mm

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Results and Discussion - DSR

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Results and Discussion - MSCR

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Results and Discussion - MSCR

From EN 16659

Tests@ 76 °C @ 70 °C @ 64 °C

160 °C 120 °C 160 °C 120 °C 160 °C 120 °C

ε1100 0.413 0.454 0.250 0.244 0.136 0.139

ε13200 15.8 16.8 9.32 9.32 4.69 4.99

R100 10.7% 8.4% 46.9% 37.5% 55.5% 45.4%

R3200 4.6% 2.2% 28.8% 13.9% 47.1% 24.3%

Rdiff 56.7% 74.2% 38.7% 62.9% 15.2% 46.6%

Jnr100 3.69 kPa-1 4.16 kPa-1 1.33 kPa-1 1.53 kPa-1 0.605 kPa-1 0.757 kPa-1

Jnr3200 4.72 kPa-1 5.15 kPa-1 2.08 kPa-1 2.51 kPa-1 0.775 kPa-1 1.18 kPa-1

Jnr-diff 27.9% 23.8% 56.8% 64.3% 28.0% 56.2%

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•  Linear viscoelastic region (@64 °C & 10 rad/s)

•  Low shear viscosity @0.001 rad/s

Results and Discussion - Additional

0.727 0.983

Cross model: 𝜂↑∗ − 𝜂↓∞↑∗ /𝜂↓0↑∗ − 𝜂↓∞↑∗  = 1/1+ (𝐾𝜔)↑𝑚  

Test  

@ 60 °C   @ 70 °C   @ 80 °C  

160°C   120°C   160°C   120°C   160°C   120°C  

Low shear viscosity (Pa·s) @0.001 rad/s  

3137   2161   1222   521   469   201  

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Summary

Sample ξ G’ @76°C & 1 rad/s R3200 @70°C R3200 @64°C …

160 °C 0 mm 134 Pa 28.8% 47.1% …

120 °C 2.356 mm 36.2 Pa 13.9% 24.3% …

•  A quantitative morphological parameter for PMB, i.e. the characteristic wavelength ξ by 2D-FFT method.

•  Controlling thermal history is a feasible and practical way to control PMB morphology based on the same material.

•  Homogenous PMB tends to store more energy during shearing and reach higher recovery after loading than a binary droplet-in-matrix.

•  More results coming soon…

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Workshop Swedish Node in Nordic Research School for Pavement Engineering

Thanks for your attention!

September 24 – 25, 2018, Hotel C, Stockholm

Presenter: Jiqing Zhu, [email protected]

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