Surface Tension of Asphalt Using AFM

Surface Tension of Asphalt using AFM
Appy Beemer, Troy Pauli, and Julie Miller
Pavement Performance Prediction Symposium

Adhesion and Cohesion in Asphalt Pavements
June 23-25, 2005
Cheyenne, WY
Overview
Definition of terms
AFM Background
Contact Mechanics Theory
Experimental Data
Analysis of Data
Conclusions
Definitions
Surface Tension
Force from the bulk molecules on a surface line of a liquid
Surface Energy
Work or energy required to create a unit of surface area of a
solid
Work of Cohesion
Work required to separate a material from itself at an
arbitrary boundary
Work of Adhesion
Work required to separate two dissimilar materials at their
interface
Munson, Bruce R., Donald F. Young, and Theodore H. Okiishi. Fundamentals of Fluid
Mechanics, 3rd ed. John Wiley & Sons, Inc. New York: 1998, p 26-28.
Importance for asphalt

Asphalt surface tension gives:
Cohesive properties
Adhesive properties
Time and temperature susceptible

Cohesive strength property may
need further investigation
Making the Measurement

Make an asphalt toluene solution
Initial solution concentration ~0.167g/mL
Spin cast solution onto a glass microscope

slide
Volume deposited to slide - 2.0L
Spin rate - 600 to 800 rpm
Roto-Film
Solution Spin
Casting Device
Filmetrics Thin-film
Measurement System
Storing Conditions
Use ~ 1.0 m films

Keep samples in dry box
Purge box with nitrogen gas
Keep samples at room temperature
The Operation of a Scanning Probe

Microscope
2
1. Red Laser
2. Quad-Photo Detector
3. Piezo-tube Scanner
4. Micro-Cantilever
Y
X
3
THERMAL STAGE Atomic Force Microscope

Quesant Q-Scope 250
AFM Force Curve Measurements

Bimorph
Cantilever
Z
Sample
Y
X
600
Z-deflection (nm)
400
200
-200
-400
-600
0
500
1000
Z-distance (nm)
1500
2000
600
Z-deflection (nm)
400
200
-200
-400
-600
0
500
1000
Z-distance (nm)
1500
2000
600
Z-deflection (nm)
400
200
-200
-400
-600
0
500
1000
Z-distance (nm)
1500
2000
600
Z-deflection (nm)
400
200
-200
-400
-600
0
500
1000
Z-distance (nm)
1500
2000
600
Z-deflection (nm)
400
200
-200
-400
-600
0
500
1000
Z-distance (nm)
1500
2000
600
Z-deflection (nm)
400
200
-200
-400
-600
0
500
1000
Z-distance (nm)
1500
2000
600
Z-deflection (nm)
400
200
Fpull off
-200
n R
-400
= W12
-600
0
500
1000
Z-distance (nm)
1500
2000
Deflection to Force
Approach
Retract
-5000
Load
Force, nN
-5500
-6000
Pull-off Force
-6500
-7000
-7500
0.0
0.5
1.0
1.5
Z-position, m
Detectors measure cantilever deflection

Spring Constant x Deflection = Force
Interested in load and pull-off force
2.0
Zero-Load Curve
-4500
Approach
Retract
-5000
Force, nN
-5500
-6000
-6500
-7000
-7500
0.0
0.5
1.0
Z-position, m
1.5
2.0
Negative-Load Curve
-4500
Approach
Retract
-5000
Force, nN
-5500
-6000
-6500
-7000
-7500
0.0
0.5
1.0
Z-position, m
1.5
2.0
R1
1
R
R2
1
R1
1
( R2 )
1
R1
R1
aH
a
R1
a = 2R/3
Viscoelastic Material
-2.5
-1.5
-0.5
0.5
1.5
2.5
-2000
-4000
-6000
300
-8000
-10000
-12000
Z position, um
250
Height, nm
Load Force, nN .
200
150
100
50
0
0
10
15
Distance, um
20
25
30
Viscoelastic Material
2000
-2.5
-1.5
-0.5
-2000
0.5
1.5
2.5
-4000
300
-6000
-8000
-10000
-12000
-14000
Z Distance, um
250
Height, nm
Load Force, nN
200
150
100
50
0
0
10
15
Distance, um
20
25
30
Contact Mechanics Model of an

Interface
Hertzian Contact between Rigid Surfaces
Shull, K. R., (Nov. 2004), shullgroup.northwestern.edu/pdfpublic/ref054.pdf
Phertz
4 E *a 3
=
3R
Frictionless, ideal contact
Contact Mechanics Model of an

Interface
At the JKR and DMT Limits
2
3R
(
)
a =
P + 3GR + 6GRP + 3GR
*
4E
3
P 0
PJKR =
PDMT
lim E * = 3 12 R
2 R /3a
= lim
4 2 R / 9 a
E * = 4 12 R
Contact Mechanics Model of

an Interface
At the JKR and DMT Limits
JKR
Adds load to the model
Does not account for adhesion outside the contact area
Large probe, very soft surface, high surface energy
DMT
Adds friction as well as load to the model
Accounts for adhesion outside the contact area
Wetting
Small probe, hard surface, low surface energy
Drift Procedure
Surface Tension,, dyne/cm .
100
90
80
70
60
50
Make contact with surface (low force)
40
Allow several force curve cycles (save each)
30
Decrease the z scan range (decrease the force)
20
Save another series of force curves
10
Repeat until no contact
0
-200
200
400
600
800
Load, P, nN
1000
1200
1400
Load-Unload Procedure
100
90
80
70
60
Increase z scan range to contact surface
50
Save force curve at initial contact

Increase the z scan range (increase the load)
40
Save force curve
30
Repeat until at desired load
20
Decrease the z range (decrease the load)
10
Save force curve

Repeat until no contact
0
-200
200
400
600
800
Load, P, nN
1000
1200
1400
AAB-1 Set
70
60
50
40
30
20
= 46.9 (Avg. 47.9)

10
0
-200
200
Load, P, nN
400
AAD-1 Set
110
100
90
80
70
60
50
40
30
= 42.7 (Avg. 45.0)
20
10
0
-100
100
200
Load, P, nN
300
400
500
AAF-1 Set
70
60
50
40
30
20
= 48.4 (Avg. 47.9)

10
0
-200
-100
100
Load, P, nN
200
300
400
AAM-1 Set
140
120
100
80
60
40
= 50.3 (Avg. 49.9)

20
0
-200
200
400
Load, P, nN
600
800
Average Surface60Tensions
50
40
30
AAB : 47.9 1.2
20
10
0
-125
-100
-75
-50
-25
Load, P, nN
25
50
50
40
30
AAB : 47.9 1.2
AAD : 45.0 2.6
20
10
0
-125
-100
-75
-50
-25
Load, P, nN
25
50
50
40
30
AAB : 47.9 1.2
AAD : 45.0 2.6
AAF : 47.7 2.2
20
10
0
-125
-100
-75
-50
-25
Load, P, nN
25
50
Average Surface 60Tensions

50
40
30
AAB
: 47.9 1.2
AAD
: 45.0 2.6
AAF
: 47.7 2.2
AAM
: 49.9 1.6
20
10
0
-125
-100
-75
-50
-25
Load, P, nN
25
50
JKR/DMT
JKR
DMT
JKR/DMT
JKR
DMT
60
50
40
30
AAB
20
AAD
AAF
10
AAM
0
-125
-100
-75
-50
-25
Load, P, nN
25
50
Average Surface Tensions

AAD-1
AAF-1
AAB-1
AAM-1
45.0
47.7
47.9
49.9
2.4
2.2
1.2
1.6
AAD-1 Neat
AAD-1 PAV 240 h
AAD-1 PAV 480 h
AAD-1 PPA & PAV 96 h
AAD-1 PPA & PAV 184 h
Least Cohesive
Most Cohesive
40.9
44.7
43.7
46.2
47.0
1.0
1.3
1.4
0.5
0.7
Least Cohesive
Most Cohesive
Wc = 2
Conclusions
Neat asphalt adhesive properties:
Long-range, wetting forces
Short-range, non-wetting forces
Neat asphalt cohesive properties

Least cohesive asphalts (AAD)
Moderately cohesive asphalts (AAB & AAF)
Most cohesive asphalts (AAM)
Modified asphalt cohesive properties

Least cohesive (Neat)
Moderately cohesion (PAV)
Most cohesive (PPA Modified)
Future Work
Explore other parameters
Temperature
Rate
Aging
Additives
Adhesion-cohesion balance
Continue to refine experimental
procedures
ACKNOWLEDGEMENTS
FHWA for their Financial Support under Contract No. DTFH6199C-00022
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Surface Tension of Asphalt Using AFM

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Surface Tension of Asphalt Using AFM

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Surface Tension of Asphalt using AFM

Appy Beemer, Troy Pauli, and Julie Miller

Pavement Performance Prediction Symposium

Importance for asphalt

Time and temperature susceptible

Making the Measurement

Spin cast solution onto a glass microscope

Use ~ 1.0 m films

The Operation of a Scanning Probe

THERMAL STAGE Atomic Force Microscope

AFM Force Curve Measurements

Detectors measure cantilever deflection

Contact Mechanics Model of an

Frictionless, ideal contact

Contact Mechanics Model of an

Contact Mechanics Model of

Small probe, hard surface, low surface energy

Make contact with surface (low force)

Allow several force curve cycles (save each)

Decrease the z scan range (decrease the force)

Save another series of force curves

Repeat until no contact

Increase z scan range to contact surface

Save force curve at initial contact

Save force curve

Repeat until at desired load

Decrease the z range (decrease the load)

Save force curve

= 46.9 (Avg. 47.9)

= 42.7 (Avg. 45.0)

= 48.4 (Avg. 47.9)

= 50.3 (Avg. 49.9)

Surface Tension,, dyne/cm .

Surface Tension,, dyne/cm .

Surface Tension,, dyne/cm .

Surface Tension,, dyne/cm .

Average Surface 60Tensions

Surface Tension,, dyne/cm .

Average Surface Tensions

Neat asphalt cohesive properties

Modified asphalt cohesive properties

FHWA for their Financial Support under Contract No. DTFH6199C-00022

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