Bitumen ldquoBee-structuresrdquo bekeken

Jeroen Besamusca

Kuwait Petroleum Research amp Technology

Hilde Soenen

Nynas NV

Hartmut Fischer

TNO Technical Science

Nicole Kringos

KTH Royal Institute of Technology

RILEM TC NBM 231

Micro-structural features in bitumen ndash surprisingly rich

Catana (bee) phase

Peri (gr around) phase

Perpetua (gr continuous) phase

reflected light microscopy images of selected bitumen

surfaces were taken using a magnification of 150x

Cooling rate ca 10 Kmin

AFM principle

Phase contrast mode

Phase imaging in AFM refers to recording the phase shift signal

in intermittent-contact AFM The phase shift can be thought of as

a ldquodelayrdquo in the oscillation of the cantilever as is moves up and

down in and out of contact with the sample The phase signal in

soft materials is sensitive to viscoelastic properties and adhesion

forces with some participation by elastic properties but also

reflects topometric differences (differences in slope) This is

because the phase is really a measure of the energy dissipation

involved in the contact between the tip and the sample

Surface Science 519 2002 L593-L598

Micro-structural features in bitumen ndash surprisingly rich

Catana (bee) phase

Peri (gr around) phase

Perpetua (gr continuous) phase

reflected light microscopy images of selected bitumen

surfaces were taken using a magnification of 150x

Cooling rate ca 10 Kmin

AFM principle

Phase contrast mode

Phase imaging in AFM refers to recording the phase shift signal

in intermittent-contact AFM The phase shift can be thought of as

a ldquodelayrdquo in the oscillation of the cantilever as is moves up and

down in and out of contact with the sample The phase signal in

soft materials is sensitive to viscoelastic properties and adhesion

forces with some participation by elastic properties but also

reflects topometric differences (differences in slope) This is

because the phase is really a measure of the energy dissipation

involved in the contact between the tip and the sample

Surface Science 519 2002 L593-L598

reflected light microscopy images of selected bitumen

surfaces were taken using a magnification of 150x

Cooling rate ca 10 Kmin

AFM principle

Phase contrast mode

Phase imaging in AFM refers to recording the phase shift signal

in intermittent-contact AFM The phase shift can be thought of as

a ldquodelayrdquo in the oscillation of the cantilever as is moves up and

down in and out of contact with the sample The phase signal in

soft materials is sensitive to viscoelastic properties and adhesion

forces with some participation by elastic properties but also

reflects topometric differences (differences in slope) This is

because the phase is really a measure of the energy dissipation

involved in the contact between the tip and the sample

Surface Science 519 2002 L593-L598

AFM principle

Phase contrast mode

Phase imaging in AFM refers to recording the phase shift signal

in intermittent-contact AFM The phase shift can be thought of as

a ldquodelayrdquo in the oscillation of the cantilever as is moves up and

down in and out of contact with the sample The phase signal in

soft materials is sensitive to viscoelastic properties and adhesion

forces with some participation by elastic properties but also

reflects topometric differences (differences in slope) This is

because the phase is really a measure of the energy dissipation

involved in the contact between the tip and the sample

Surface Science 519 2002 L593-L598

Handling bitumen Difficulty ndash bitumen is a very good glue and displays a Tg of about ndash 15 ordmC

so the material is visco-elastic at ambient temperatureshellip

Preparation on steel disks at

100 ordmC to get smooth surface

and subsequent cooling and

annealing at rt all samples

Q8 70100

Images immediately after 24 hrs and after 3 weeks of annealing

Different grades and origin ndash similar features

North Sea

Q 8 Q 8 Venezuela

REB

Middle

East

Effects of cooling rate Not only annealing also cooling rate can influence observable structural features ndash

fast quenching leads to early crystallisation of paraffinic componentshellip

Cooling rates are approx 50 Kmin

Overview of samples of the RR-study within the TC NBM 231

Code Supplier Bitumen Pen dmm RampK degC Wax percentage

volgens EN 12606-1

Bit-A Nynas 70100 91 462 03

Bit-B Nynas 70100 86 464 17

Bit-C Q8 70100 82 458 1

Bit-D Nynas Bit-A +3 sasobit 50 78 -

H Soenen J Besamusca LD Poulikakos J-P Planche P Das N Kringos J Grenfell E Chailleux (2013) Differential Scanning Calorimetry

applied to bitumen Results of the RILEM NBM TG1 Round Robin test Challenges While Performing AFM on Bitumen N Kringos et al (Eds)

Multi-Scale Model amp Charact of Infrastruct Mater RILEM 8 311

H Fischer LD Poulikakos J-P Planche P Das J Grenfell (2013) Challenges while performing AFM on Bitumen Challenges While Performing

AFM on Bitumen N Kringos et al (Eds) Multi-Scale Model amp Charact of Infrastruct Mater RILEM 8 89ndash98

Soenen H Besamusca J Fischer HR Poulikakos LD Planche J-P Das PK Kringos N Grenfell JRA Lu X Chailleux E

Laboratory investigation of bitumen based on round robin DSC and AFM tests (2013) Materials and StructuresMateriaux et Constructions 1-16

Typical pictures obtained from the different sampleshellip

Bitumen A

featureless

Bitumen B

Bitumen D Bitumen C

All three other

samples show

typical micro-

structural

features

ldquoBeersquosrdquo

Round-robin test on Atomic Force Microscopy (AFM)

bull Sample size (weight) 15-30 mg Bitumen film on (heat) conductive sample holder

bull Temperature history preparation at 110 ndash 130degC to let the binder level out for 15 minutes

than conditioning at rt for 24 hrs before test

bull Test temperature 25degC (controlled)

bull Scan rate 1Hz

bull Cantilever Spring constant ~ 40Nm resonant frequency ~ 300 kHz

bull Image type topography and phase size 50μm times 50 μm and 15μm times 15 μm

Bitumen C Q 8 70100

rt 40 ordmC 45 ordmC 50 ordmC

60 ordmC 55 ordmC 65 ordmC

Structural changes upon heating (Bitumen C)

DSC enables detection of glass transition temperature and meltingcrystallisation features

Bitumen A just Tg Bitumen C Tg and several melting events

Measurement of melting enthalphy possible

Very good reproducibility of experiments within the RR test

Linking structural changes to thermal effects by Temperature dependent experiments

catana catana

Quantification of changes by analyzing area distribution of the different phases in phase contrast pictures

Q8 70 - 100

022

024

026

028

030

032

034

036

0

01

02

03

04

05

06

07

08

0 10 20 30 40 50 60 70 80

he

at

flo

w (

Wg

)

are

a p

art

Temperature (oC)

Catana-phase

Peri-phase

Perpetua-phase

DSC

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

Different grades and origin ndash similar features

North Sea

Q 8 Q 8 Venezuela

REB

Middle

East

Effects of cooling rate Not only annealing also cooling rate can influence observable structural features ndash

fast quenching leads to early crystallisation of paraffinic componentshellip

Cooling rates are approx 50 Kmin

Overview of samples of the RR-study within the TC NBM 231

Code Supplier Bitumen Pen dmm RampK degC Wax percentage

volgens EN 12606-1

Bit-A Nynas 70100 91 462 03

Bit-B Nynas 70100 86 464 17

Bit-C Q8 70100 82 458 1

Bit-D Nynas Bit-A +3 sasobit 50 78 -

H Soenen J Besamusca LD Poulikakos J-P Planche P Das N Kringos J Grenfell E Chailleux (2013) Differential Scanning Calorimetry

applied to bitumen Results of the RILEM NBM TG1 Round Robin test Challenges While Performing AFM on Bitumen N Kringos et al (Eds)

Multi-Scale Model amp Charact of Infrastruct Mater RILEM 8 311

H Fischer LD Poulikakos J-P Planche P Das J Grenfell (2013) Challenges while performing AFM on Bitumen Challenges While Performing

AFM on Bitumen N Kringos et al (Eds) Multi-Scale Model amp Charact of Infrastruct Mater RILEM 8 89ndash98

Soenen H Besamusca J Fischer HR Poulikakos LD Planche J-P Das PK Kringos N Grenfell JRA Lu X Chailleux E

Laboratory investigation of bitumen based on round robin DSC and AFM tests (2013) Materials and StructuresMateriaux et Constructions 1-16

Typical pictures obtained from the different sampleshellip

Bitumen A

featureless

Bitumen B

Bitumen D Bitumen C

All three other

samples show

typical micro-

structural

features

ldquoBeersquosrdquo

Round-robin test on Atomic Force Microscopy (AFM)

bull Sample size (weight) 15-30 mg Bitumen film on (heat) conductive sample holder

bull Temperature history preparation at 110 ndash 130degC to let the binder level out for 15 minutes

than conditioning at rt for 24 hrs before test

bull Test temperature 25degC (controlled)

bull Scan rate 1Hz

bull Cantilever Spring constant ~ 40Nm resonant frequency ~ 300 kHz

bull Image type topography and phase size 50μm times 50 μm and 15μm times 15 μm

Bitumen C Q 8 70100

rt 40 ordmC 45 ordmC 50 ordmC

60 ordmC 55 ordmC 65 ordmC

Structural changes upon heating (Bitumen C)

DSC enables detection of glass transition temperature and meltingcrystallisation features

Bitumen A just Tg Bitumen C Tg and several melting events

Measurement of melting enthalphy possible

Very good reproducibility of experiments within the RR test

Linking structural changes to thermal effects by Temperature dependent experiments

catana catana

Quantification of changes by analyzing area distribution of the different phases in phase contrast pictures

Q8 70 - 100

022

024

026

028

030

032

034

036

0

01

02

03

04

05

06

07

08

0 10 20 30 40 50 60 70 80

he

at

flo

w (

Wg

)

are

a p

art

Temperature (oC)

Catana-phase

Peri-phase

Perpetua-phase

DSC

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

Effects of cooling rate Not only annealing also cooling rate can influence observable structural features ndash

fast quenching leads to early crystallisation of paraffinic componentshellip

Cooling rates are approx 50 Kmin

Overview of samples of the RR-study within the TC NBM 231

Code Supplier Bitumen Pen dmm RampK degC Wax percentage

volgens EN 12606-1

Bit-A Nynas 70100 91 462 03

Bit-B Nynas 70100 86 464 17

Bit-C Q8 70100 82 458 1

Bit-D Nynas Bit-A +3 sasobit 50 78 -

H Soenen J Besamusca LD Poulikakos J-P Planche P Das N Kringos J Grenfell E Chailleux (2013) Differential Scanning Calorimetry

applied to bitumen Results of the RILEM NBM TG1 Round Robin test Challenges While Performing AFM on Bitumen N Kringos et al (Eds)

Multi-Scale Model amp Charact of Infrastruct Mater RILEM 8 311

H Fischer LD Poulikakos J-P Planche P Das J Grenfell (2013) Challenges while performing AFM on Bitumen Challenges While Performing

AFM on Bitumen N Kringos et al (Eds) Multi-Scale Model amp Charact of Infrastruct Mater RILEM 8 89ndash98

Soenen H Besamusca J Fischer HR Poulikakos LD Planche J-P Das PK Kringos N Grenfell JRA Lu X Chailleux E

Laboratory investigation of bitumen based on round robin DSC and AFM tests (2013) Materials and StructuresMateriaux et Constructions 1-16

Typical pictures obtained from the different sampleshellip

Bitumen A

featureless

Bitumen B

Bitumen D Bitumen C

All three other

samples show

typical micro-

structural

features

ldquoBeersquosrdquo

Round-robin test on Atomic Force Microscopy (AFM)

bull Sample size (weight) 15-30 mg Bitumen film on (heat) conductive sample holder

bull Temperature history preparation at 110 ndash 130degC to let the binder level out for 15 minutes

than conditioning at rt for 24 hrs before test

bull Test temperature 25degC (controlled)

bull Scan rate 1Hz

bull Cantilever Spring constant ~ 40Nm resonant frequency ~ 300 kHz

bull Image type topography and phase size 50μm times 50 μm and 15μm times 15 μm

Bitumen C Q 8 70100

rt 40 ordmC 45 ordmC 50 ordmC

60 ordmC 55 ordmC 65 ordmC

Structural changes upon heating (Bitumen C)

DSC enables detection of glass transition temperature and meltingcrystallisation features

Bitumen A just Tg Bitumen C Tg and several melting events

Measurement of melting enthalphy possible

Very good reproducibility of experiments within the RR test

Linking structural changes to thermal effects by Temperature dependent experiments

catana catana

Quantification of changes by analyzing area distribution of the different phases in phase contrast pictures

Q8 70 - 100

022

024

026

028

030

032

034

036

0

01

02

03

04

05

06

07

08

0 10 20 30 40 50 60 70 80

he

at

flo

w (

Wg

)

are

a p

art

Temperature (oC)

Catana-phase

Peri-phase

Perpetua-phase

DSC

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

Overview of samples of the RR-study within the TC NBM 231

Code Supplier Bitumen Pen dmm RampK degC Wax percentage

volgens EN 12606-1

Bit-A Nynas 70100 91 462 03

Bit-B Nynas 70100 86 464 17

Bit-C Q8 70100 82 458 1

Bit-D Nynas Bit-A +3 sasobit 50 78 -

H Soenen J Besamusca LD Poulikakos J-P Planche P Das N Kringos J Grenfell E Chailleux (2013) Differential Scanning Calorimetry

applied to bitumen Results of the RILEM NBM TG1 Round Robin test Challenges While Performing AFM on Bitumen N Kringos et al (Eds)

Multi-Scale Model amp Charact of Infrastruct Mater RILEM 8 311

H Fischer LD Poulikakos J-P Planche P Das J Grenfell (2013) Challenges while performing AFM on Bitumen Challenges While Performing

AFM on Bitumen N Kringos et al (Eds) Multi-Scale Model amp Charact of Infrastruct Mater RILEM 8 89ndash98

Soenen H Besamusca J Fischer HR Poulikakos LD Planche J-P Das PK Kringos N Grenfell JRA Lu X Chailleux E

Laboratory investigation of bitumen based on round robin DSC and AFM tests (2013) Materials and StructuresMateriaux et Constructions 1-16

Typical pictures obtained from the different sampleshellip

Bitumen A

featureless

Bitumen B

Bitumen D Bitumen C

All three other

samples show

typical micro-

structural

features

ldquoBeersquosrdquo

Round-robin test on Atomic Force Microscopy (AFM)

bull Sample size (weight) 15-30 mg Bitumen film on (heat) conductive sample holder

bull Temperature history preparation at 110 ndash 130degC to let the binder level out for 15 minutes

than conditioning at rt for 24 hrs before test

bull Test temperature 25degC (controlled)

bull Scan rate 1Hz

bull Cantilever Spring constant ~ 40Nm resonant frequency ~ 300 kHz

bull Image type topography and phase size 50μm times 50 μm and 15μm times 15 μm

Bitumen C Q 8 70100

rt 40 ordmC 45 ordmC 50 ordmC

60 ordmC 55 ordmC 65 ordmC

Structural changes upon heating (Bitumen C)

DSC enables detection of glass transition temperature and meltingcrystallisation features

Bitumen A just Tg Bitumen C Tg and several melting events

Measurement of melting enthalphy possible

Very good reproducibility of experiments within the RR test

Linking structural changes to thermal effects by Temperature dependent experiments

catana catana

Quantification of changes by analyzing area distribution of the different phases in phase contrast pictures

Q8 70 - 100

022

024

026

028

030

032

034

036

0

01

02

03

04

05

06

07

08

0 10 20 30 40 50 60 70 80

he

at

flo

w (

Wg

)

are

a p

art

Temperature (oC)

Catana-phase

Peri-phase

Perpetua-phase

DSC

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

Typical pictures obtained from the different sampleshellip

Bitumen A

featureless

Bitumen B

Bitumen D Bitumen C

All three other

samples show

typical micro-

structural

features

ldquoBeersquosrdquo

Round-robin test on Atomic Force Microscopy (AFM)

bull Sample size (weight) 15-30 mg Bitumen film on (heat) conductive sample holder

bull Temperature history preparation at 110 ndash 130degC to let the binder level out for 15 minutes

than conditioning at rt for 24 hrs before test

bull Test temperature 25degC (controlled)

bull Scan rate 1Hz

bull Cantilever Spring constant ~ 40Nm resonant frequency ~ 300 kHz

bull Image type topography and phase size 50μm times 50 μm and 15μm times 15 μm

Bitumen C Q 8 70100

rt 40 ordmC 45 ordmC 50 ordmC

60 ordmC 55 ordmC 65 ordmC

Structural changes upon heating (Bitumen C)

DSC enables detection of glass transition temperature and meltingcrystallisation features

Bitumen A just Tg Bitumen C Tg and several melting events

Measurement of melting enthalphy possible

Very good reproducibility of experiments within the RR test

Linking structural changes to thermal effects by Temperature dependent experiments

catana catana

Quantification of changes by analyzing area distribution of the different phases in phase contrast pictures

Q8 70 - 100

022

024

026

028

030

032

034

036

0

01

02

03

04

05

06

07

08

0 10 20 30 40 50 60 70 80

he

at

flo

w (

Wg

)

are

a p

art

Temperature (oC)

Catana-phase

Peri-phase

Perpetua-phase

DSC

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

Round-robin test on Atomic Force Microscopy (AFM)

bull Sample size (weight) 15-30 mg Bitumen film on (heat) conductive sample holder

bull Temperature history preparation at 110 ndash 130degC to let the binder level out for 15 minutes

than conditioning at rt for 24 hrs before test

bull Test temperature 25degC (controlled)

bull Scan rate 1Hz

bull Cantilever Spring constant ~ 40Nm resonant frequency ~ 300 kHz

bull Image type topography and phase size 50μm times 50 μm and 15μm times 15 μm

Bitumen C Q 8 70100

rt 40 ordmC 45 ordmC 50 ordmC

60 ordmC 55 ordmC 65 ordmC

Structural changes upon heating (Bitumen C)

DSC enables detection of glass transition temperature and meltingcrystallisation features

Bitumen A just Tg Bitumen C Tg and several melting events

Measurement of melting enthalphy possible

Very good reproducibility of experiments within the RR test

Linking structural changes to thermal effects by Temperature dependent experiments

catana catana

Quantification of changes by analyzing area distribution of the different phases in phase contrast pictures

Q8 70 - 100

022

024

026

028

030

032

034

036

0

01

02

03

04

05

06

07

08

0 10 20 30 40 50 60 70 80

he

at

flo

w (

Wg

)

are

a p

art

Temperature (oC)

Catana-phase

Peri-phase

Perpetua-phase

DSC

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

Bitumen C Q 8 70100

rt 40 ordmC 45 ordmC 50 ordmC

60 ordmC 55 ordmC 65 ordmC

Structural changes upon heating (Bitumen C)

DSC enables detection of glass transition temperature and meltingcrystallisation features

Bitumen A just Tg Bitumen C Tg and several melting events

Measurement of melting enthalphy possible

Very good reproducibility of experiments within the RR test

Linking structural changes to thermal effects by Temperature dependent experiments

catana catana

Quantification of changes by analyzing area distribution of the different phases in phase contrast pictures

Q8 70 - 100

022

024

026

028

030

032

034

036

0

01

02

03

04

05

06

07

08

0 10 20 30 40 50 60 70 80

he

at

flo

w (

Wg

)

are

a p

art

Temperature (oC)

Catana-phase

Peri-phase

Perpetua-phase

DSC

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

DSC enables detection of glass transition temperature and meltingcrystallisation features

Bitumen A just Tg Bitumen C Tg and several melting events

Measurement of melting enthalphy possible

Very good reproducibility of experiments within the RR test

Linking structural changes to thermal effects by Temperature dependent experiments

catana catana

Quantification of changes by analyzing area distribution of the different phases in phase contrast pictures

Q8 70 - 100

022

024

026

028

030

032

034

036

0

01

02

03

04

05

06

07

08

0 10 20 30 40 50 60 70 80

he

at

flo

w (

Wg

)

are

a p

art

Temperature (oC)

Catana-phase

Peri-phase

Perpetua-phase

DSC

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

Very good reproducibility of experiments within the RR test

Linking structural changes to thermal effects by Temperature dependent experiments

catana catana

Quantification of changes by analyzing area distribution of the different phases in phase contrast pictures

Q8 70 - 100

022

024

026

028

030

032

034

036

0

01

02

03

04

05

06

07

08

0 10 20 30 40 50 60 70 80

he

at

flo

w (

Wg

)

are

a p

art

Temperature (oC)

Catana-phase

Peri-phase

Perpetua-phase

DSC

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

Linking structural changes to thermal effects by Temperature dependent experiments

catana catana

Quantification of changes by analyzing area distribution of the different phases in phase contrast pictures

Q8 70 - 100

022

024

026

028

030

032

034

036

0

01

02

03

04

05

06

07

08

0 10 20 30 40 50 60 70 80

he

at

flo

w (

Wg

)

are

a p

art

Temperature (oC)

Catana-phase

Peri-phase

Perpetua-phase

DSC

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

catana catana

Quantification of changes by analyzing area distribution of the different phases in phase contrast pictures

Q8 70 - 100

022

024

026

028

030

032

034

036

0

01

02

03

04

05

06

07

08

0 10 20 30 40 50 60 70 80

he

at

flo

w (

Wg

)

are

a p

art

Temperature (oC)

Catana-phase

Peri-phase

Perpetua-phase

DSC

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

022

024

026

028

030

032

034

036

0

01

02

03

04

05

06

07

08

0 10 20 30 40 50 60 70 80

he

at

flo

w (

Wg

)

are

a p

art

Temperature (oC)

Catana-phase

Peri-phase

Perpetua-phase

DSC

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

bull Het onderzoek in verschillende laboratoria lijdt tot vergelijkbare resultaten De

combinatie AFM en DSC metingen toont een relatie tussen de aanwezigheid

van ldquobee-structurenrdquo en de aanwezigheid van kristallijn materiaal (Bit A vs Bit

B-D)

bull Bij opwarmen verdwijnen de bee-structuren geleidelijk terwijl ook de kristallijne

structuren een breed smeltgedrag vertonen

bull Uit DSC metingen blijkt dat de termische voorgeschiedenis van het sample een

belangrijke invloed heeft op de vorm van de smeltcurve (bitumina die kristallijn

materiaal bevatten

bull De mid temperatuur van de glasovergang en de piek temperatuur van het

smeltsignaal kunnen met een goede reproduceerbaarheid gemeten worden

bull De reproduceerbaarheid voor enthalpie is voorlopig niet goed metingen na

andere en langere annealingsperioden zouden dit mogelijks verbeteren

Conclusies Round-robin test

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

Quantification of micro-structure mechanics by PFT QNM - also temperature dependent

Catanaperi phase is harder perpetua

phase more viscous and sticky Hysteresis

in mechanics with respect to temperaturehellip

Fischer HR Stadler H Erina N (2013)

J Microscopy 250

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

Quantification of wetting behaviour onto different aggregate surface chemistries

Surprising result Catanaperi-

phase wets all used surfaces

(limestone clay quartz) better [1]

Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

Quantification of wetting behaviour onto different aggregate surface chemistries

Preferred wetting of Catanaperi-phase [2]

This is most likely related to

asphaltene precipitation

Early results of asphaltene

precipitation on stones

Existence of asphalthenes in

Catanaperi phase Fischer HR Dillingh EC Hermse CGM

(2013) Appl Surface Sci 265 495-499

θ

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

And now the real challenge ndash AFM on asphalt

Aggregate particle

Bituminous binder

Also here phase separation

and microstructures as well

as crystalline paraffin

domains present

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support

Acknowledgements

and for the supply of bitumen

Patrick Markus Hartmut Stadler and Natalia Erina for support

and PFT QNM and

RILEM technical committee (TC) on nano bituminous materials NBM 231

Lily D Poulikakos (EMPA) Jean-Pascal Planche (WRI) Prabir Das

(KTH) James Grenfell (University of Nottingham) Emmanuel Chailleux

(IFSTTAR) Xiaohu Lu (Nynas)

for financial support