Nano-Rheology/Nano-Mechanics and Scanning Probe Microscope Imaging Based on Novel

Transcription

1 Nano-Rheology/Nano-Mechanics and Scanning Probe Microscope Imaging Based on Novel Sample Preparation Techniques Will Grimes, Bill Tuminello, Ryan Boysen, James Beiswenger, Jerry Forney, Niki Ki Kringos, and dtroy Pauli PAVEMENT PERFORMANCE PREDICTION SYMPOSIUM Hilton Garden Inn and University of Wyoming Conference Center Laramie, Wyoming, July 15, 2010

2 Acknowledgements The authors gratefully acknowledge the Federal Highway Administration, U.S. Department of Transportation for financial support of this research under Contract No s., DFTH61-07-D D and DFTH61-07-H H 00009

3 Outline Theory A Reversible Rate Mechanism Diffuse Interface Theory Experiments SARA Fractionation at o HP-GPC (high performance gel permeation chromatography) SimDis-TGA (thermogravimetric analyses) Ultrasound (temperature-fluidity) AFM (phase separation phenomena) Results Discussion Conclusions

4 Theory

5 Thermodynamically Based Fracture and Self-Healing Theory Phase Field Description of Wax Crystallization in Asphalt

6 Phase Field Description of Wax Crystallization in Asphalt total crys wall ve crys fmix (, ) d f ( ) da wall w ve f d d

7 Rate Expression: Wax Crystallization in Asphalt 2 d t d Feng, J.J., Liu, C., Shen, J. and Yue, P., An energetic variational formulation with phase field methods for interfacial dynamics of complex fluids: Advantages and challenges. Modeling of soft matter, 141, 1-26, New York: Springer. Zhou, C., Yue, P., Fang, J.J., Ollivier-Gooch, C.F. and Hu, H.H., D phase-field simulations of interfacial dynamics in Newtonian and viscoelastic fluids. J. computational physics, 229, Yue, P., Zhou, C., Feng, J.J., Ollivier-Gooch, C.F. and Hu, H.H., Phase-field simulations of interfacial dynamics in viscoelastic fluids using finite elements with adaptive mesh, J. computational physics, 219,

8 Phase-Field Rate Expression for Diffuse Fracture and Crack Solidification i (Self-Healing) li D 2 t u k m(, ) m (, T) m o ( 0) k i i i t 2 d d

9 Phase-Field Rate Expression for Diffuse Fracture (Repeated Loading) and Crack Solidification i (Self-Healing) li m k (, ) mi ( i ) k m (, T ) m ( ) m i i i i k (, ) m ( ) i i j j Healing Efficiency m ( ) m ( ) n n η mn( n)

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11 Experiments

12 SARA Chromatography Saturates Aromatics Resins Asphaltenesp

13 Molecular Weight/Size Determination: High Performance Gel Permeation Chromatography (HP-GPS)

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15 HP-GPS (High Performance-Gel GlPermeation Chromatography) h) Determination of Mobility, Thermal Dilatometry a K M w K n dn 4 dc a log 2 K RIresponce M w

16 M Mc c w i i i M c c M n i i i 2 M z Mi ci Mi ci w n a' log /100 2 n M w Asphalt M p (Da) M w (Da) M n (Da) M z (Da) w n n (mvml) a ' AAA-1 AAB-1 AAC-1 AAD-1 AAF-1 AAG-1 AAK-1 AAM-1 MN1-2 MN1-3 MN1-4 MN1-5 AZ1-1 AZ1-2 AZ1-3 AZ

17 Vaporization Temperature: Thermo Gravimetric Analysis (TGA) Goodrum, J. W. ande E. M. Siesel, 1996, Thermogravimetricanalysisforboilingpointsand analysis and vaporpressure pressure. Journal of Thermal Analysis and Calorimetry, 46(5), Goodrum, J. W., 2002, Volatility and boiling points of biodiesel from vegetable oils and tallow. Biomass and Bioenergy, 22(3), Goodrum, J. W., and D. P. Geller, 2002, Rapid thermogravimetric measurements of boiling points and vapor pressure of saturated medium- and long-chain triglycerides. Bioresource Technology, 84(1), Yuan, W., A.C. Hansen, Q. Zhang, 2005, Vapor pressure and normal boiling point predictions for pure methyl esters and biodiesel fuels. Fuel, 84 (2005)

18 Weig ght % Pyrolysis Carbon Burn Off Pyrolysis Time, t p (@ 20 C/min), (min)

19 35 Saturates Deriv. Wt t. (%/Min) Napthene Aromatics Polar Aromatics Neat Pyrolysis Volatiles Heating Rate 20 C/Min Ambient 600 C Carbon Burn Off Temperature ( C)

20 f( x, x,,, ) x x0, x x0 1 x x0, e 1/ ( 1)/ 1 x x0 1

21 Single Wavelength Ultrasound Spectroscopy

22 The speed of the sound wave through a material is proportional to wavelength and frequency and will be dampened slowed dependent on the solid-fluid quality of the material.

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25 Atomic Force Microscopy

26 Automated Spin-Casting Apparatus

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28 Results and Discussion

29 Figure 1b. WM-AFM topography scans (40x40-m) of eight SHRP asphalts images after Figure 1a. WM-AFM topography scans (40x40-m) of eight SHRP asphalts images after spincasting and drying. Left-to-right, from top to bottom: AAA-1, AAB-1, AAC-1, AAD-1 AAF-1, AAF-1, AAG-1, AAK-1, and AAM-1. AAG-1, AAK-1, and AAM-1. thermal conditioning. Left-to-right, from top to bottom: AAA-1, AAB-1, AAC-1, AAD-1,

30 a. b. c. d. Figure 8. WM-AFM topography scans (40x40-m) of AAA-1doped with 2% ( a) octacosane, (b) tetratetracontane, (c) (100x100-m) pentacontane and (d) 2% (IGI 5788A) microcrystalline wax.

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34 SAT% NA% SAT % NA % SAT % NA % T T ( SAT) T ( NA) max w max max Asphalt %SAT %NA T max K, SAT T max K, NA T, max w K, SAT+NA AAA-1 AAB-1 AAC-1 AAD-1 AAF-1 AAK-1 AAG-1 AAM MN1-4 MN1-5 MN1-2 MN1-3 AZ-1 AZ-2 AZ-3 AZ-4 34% 28% 37% 40% 26% 25% 32% 23% % 32% 32% 33% 26% 17% 22% 25% 66% 72% 63% 60% 74% 75% 68% 77% % 68% 68% 67% 74% 83% 78% 75%

35 SAT % NA% SAT % NA % SAT % NA % M p M p( SAT) M p( NA) w SAT NA SAT NA Asphalt %SAT %NA M p, SAT(Da) M p, NA(Da) M p w,sat+na(da) AAA-1 AAB-1 AAC-1 AAD-1 AAF-1 AAK-1 AAG-1 AAM MN1-4 MN1-5 MN1-2 MN1-3 AZ-2 AZ-1 AZ-3 AZ-4 34% 28% 37% 40% 26% 25% 32% 23% % 32% 32% 33% 26% 17% 22% 25% 66% 72% 63% 60% 74% 75% 68% 77% % 68% 68% 67% 74% 83% 78% 75%

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39 MN1 2 neat PHASE MN1 3 Neat PHASE MN1 4 Neat PHASE 250 Transverse Crack king (LF) Aug 5 May MN1 5 neat PHASE 0 MN1 2 MN1 3 MN1 4 MN1 5 Asphalt

40 SAT % NA% SAT % NA % SAT % NA % M p M p( SAT) M p( NA) w SAT NA SAT NA Asphalt %SAT %NA M p,sat(da) M p,na(da) M p w,sat+na(da) AAA-1 AAB-1 AAC-1 AAD-1 AAF-1 AAK-1 AAG-1 AAM MN-4 MN-5 MN-2 MN-3 AZ-1 AZ-2 AZ-3 AZ-4 34% 28% 37% 40% 26% 25% 32% 23% % 32% 32% 33% 26% 17% 22% 25% 66% 72% 63% 60% 74% 75% 68% 77% % 68% 68% 67% 74% 83% 78% 75%

41 Crack map data AZ Asphalt Fatigue Cracking, m 2 Longitudinal Cracking Wheel path, m Longitudinal Cracking non-wheel path, m Transverse Cracking, m AZ1-1 AZ1-2 AZ1-3 AZ

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43 SAT % NA% SAT % NA % SAT % NA % M p M p( SAT) M p( NA) w SAT NA SAT NA Asphalt %SAT %NA M p,sat(da) M p,na(da) M p w,sat+na(da) AAA-1 AAB-1 AAC-1 AAD-1 AAF-1 AAK-1 AAG-1 AAM MN-4 MN-5 MN-2 MN-3 AZ-1 AZ-2 AZ-3 AZ-4 34% 28% 37% 40% 26% 25% 32% 23% % 32% 32% 33% 26% 17% 22% 25% 66% 72% 63% 60% 74% 75% 68% 77% % 68% 68% 67% 74% 83% 78% 75%

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46 Novel Sample Preparation and Investigation i Techniques by Atomic Force Microscopy

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49 wg fract AAK 6

50 wg fract AAK 6 wg fract AAK 6

51 wg fract AAK 14 a

52 wg fract AAA 4

53 wg fract AAC 2 c

54 wg fract AAD 1 c

55 wg fract AAG 3 c

56 wg fract AAC 7 b

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58 Nano-Rheology Nano Rheology by Atomic Force Microscopy

59 Multi-Scanners Configuration: AFM Scanner Head and nano-positioning stage

60 Nano-rheology: Theory G ( ) F * R Oscillating Force F(t) () Probe of Radius R liquid drop G * ( ) F 0 R h h Oscillating Plate: h rigid backing is the complex modulus of the test liquid as a function of frequency in N/m 2 = Pa is the amplitude of the sinusoidal oscillation force felt by the probe, in Newtons (N) is the probe radius in meters (m) is the amplitude of the probe s oscillation E. Pelletier, J.P. Montfort, J.L. Loubet, A. Tonck, J.M. George, Dynamics of Compressed Polymer Layers Absorbed on Solid Surfaces, Macromolecules 1995, 28,

61 Stage/Detector Movement for Probe Resting on Glass Plate Stage Probe y = *t *sine(0.0975*t ) - detector y = *sine(0.0975*t ) - stage Time(sec)

62 y Asin( t ) Stage/Detector Movement for 57 Pa s Viscosity Standard at 25 C Stage(volts) Detector(volts) y = *sin(9.46*t ) - stage y = *sin(9.46*t ) - detector time(sec)

63 Conclusions A phase field based diffuse interface theory is proposed to conceptually study fracture-healing kinetics in a reaction mechanism frame work applicable to asphalt pavements. The wax-oil properties of asphalt provide moving parts or a chemomechanical mechanism to facilitate fracture/self-healing. Molecular weight distributions of wax-oil components of asphalt appear to be linked to fracture/self-healing propensities, Several test methods were presented which characterize the compositional property differences among asphalts derived from different sources relevant to fracture and healing. Future work entails comprehensive characterization of asphalt composition as input parameters to the theory/model considered.