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

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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

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-00005 D 00005 and DFTH61-07-H-00009. H 00009

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

Theory

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

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

Rate Expression: Wax Crystallization in Asphalt 2 d t d Feng, J.J., Liu, C., Shen, J. and Yue, P., 2005. 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., 2010. 3D phase-field simulations of interfacial dynamics in Newtonian and viscoelastic fluids. J. computational physics, 229, 498-511. Yue, P., Zhou, C., Feng, J.J., Ollivier-Gooch, C.F. and Hu, H.H., 2006. Phase-field simulations of interfacial dynamics in viscoelastic fluids using finite elements with adaptive mesh, J. computational physics, 219, 47-67.

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

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)

Experiments

SARA Chromatography Saturates Aromatics Resins Asphaltenesp

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

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

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 AZ1-4 848 1079 1188 703 1118 987 822 1311 896 859 971 795 1437 929 1035 915 788 816 1024 599 852 757 671 965 790 769 852 748 1200 809 876 807 991 1102 1253 778 1153 1034 911 1373 973 936 1029 912 1453 983 1073 982 1291 1428 1522 1000 1498 1356 1211 1851 1201 1143 1243 1125 1719 1192 1303 1194 1.26 1.35 1.22 1.30 1.35 1.37 1.36 1.42 1.23 1.22 121 1.21 1.22 1.21 1.22 1.22 1.22 224 169 204 172 168 183 175 171 172 179 158 168 172 171 165 162 51 51 58 39 49 45 42 55 41 41 44 36 53 41 44 40 0.34 0.41 0.37 0.39 0.41 0.38 0.39 0.41 0.38 0.37 041 0.41 0.37 0.40 0.38 0.40 0.40

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), 1251-1258. Goodrum, J. W., 2002, Volatility and boiling points of biodiesel from vegetable oils and tallow. Biomass and Bioenergy, 22(3), 205-211. 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), 75-80. 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) 943 950.

Weig ght % 100 90 80 70 60 50 40 30 20 10 0 Pyrolysis Carbon Burn Off 0 10 20 30 40 50 Pyrolysis Time, t p (@ 20 C/min), (min)

35 Saturates Deriv. Wt t. (%/Min) 30 25 20 15 Napthene Aromatics Polar Aromatics Neat Pyrolysis Volatiles Heating Rate 20 C/Min Ambient 600 C Carbon Burn Off 10 5 0 0 200 400 600 800 Temperature ( C)

f( x, x,,, ) 0 1 1 x x0, 0 1 1 1 1 1 x x0 1 x x0, e 1/ ( 1)/ 1 x x0 1

Single Wavelength Ultrasound Spectroscopy

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.

Atomic Force Microscopy

Automated Spin-Casting Apparatus

Results and Discussion

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,

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.

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-1 ------------- MN1-4 MN1-5 MN1-2 MN1-3 AZ-1 AZ-2 AZ-3 AZ-4 34% 28% 37% 40% 26% 25% 32% 23% ------------- 34% 32% 32% 33% 26% 17% 22% 25% 66% 72% 63% 60% 74% 75% 68% 77% ------------- 66% 68% 68% 67% 74% 83% 78% 75% 304 378 399 262 368 273 375 431 -------------------- 362 310 365 340 452 356 389 347 406 430 447 315 449 402 422 475 ------------------- 432 392 421 405 462 422 443 432 371 415 429 294 428 370 407 465 ------------------------- 408 366 403 384 459 411 431 411

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-1 ------------- MN1-4 MN1-5 MN1-2 MN1-3 AZ-2 AZ-1 AZ-3 AZ-4 34% 28% 37% 40% 26% 25% 32% 23% ---------- 34% 32% 32% 33% 26% 17% 22% 25% 66% 72% 63% 60% 74% 75% 68% 77% ---------- 66% 68% 68% 67% 74% 83% 78% 75% 848 1079 1188 703 1118 987 822 1311 ----------------- 971 795 896 859 1437 929 1035 915 752 916 969 630 829 750 741 1573 ------------------ 966 754 875 836 1387 939 991 883 785 962 1050 659 904 809 767 1513 ---------------------- 968 767 882 844 1400 937 1001 891

MN1 2 neat PHASE MN1 3 Neat PHASE MN1 4 Neat PHASE 250 Transverse Crack king (LF) 200 150 100 50 8 Aug 5 May MN1 5 neat PHASE 0 MN1 2 MN1 3 MN1 4 MN1 5 Asphalt

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-1 ------------- MN-4 MN-5 MN-2 MN-3 AZ-1 AZ-2 AZ-3 AZ-4 34% 28% 37% 40% 26% 25% 32% 23% ---------- 34% 32% 32% 33% 26% 17% 22% 25% 66% 72% 63% 60% 74% 75% 68% 77% ---------- 66% 68% 68% 67% 74% 83% 78% 75% 848 1079 1188 703 1118 987 822 1311 ----------------- 971 795 896 859 1437 929 1035 915 752 916 969 630 829 750 741 1573 ------------------ 966 754 875 836 1387 939 991 883 785 962 1050 659 904 809 767 1513 ---------------------- 968 767 882 844 1400 937 1001 891

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 AZ1-4 1.9 1.7 12.2 15.8 58.4 12 10.2 4.7 205.2 83.4 8.3 74.9 12.6 0.2 0.5 33.4

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-1 ------------- MN-4 MN-5 MN-2 MN-3 AZ-1 AZ-2 AZ-3 AZ-4 34% 28% 37% 40% 26% 25% 32% 23% ---------- 34% 32% 32% 33% 26% 17% 22% 25% 66% 72% 63% 60% 74% 75% 68% 77% ---------- 66% 68% 68% 67% 74% 83% 78% 75% 848 1079 1188 703 1118 987 822 1311 ----------------- 971 795 896 859 1437 929 1035 915 752 916 969 630 829 750 741 1573 ------------------ 966 754 875 836 1387 939 991 883 785 962 1050 659 904 809 767 1513 ---------------------- 968 767 882 844 1400 937 1001 891

Novel Sample Preparation and Investigation i Techniques by Atomic Force Microscopy

wg1265 78 fract AAK 6

wg1265 78 fract AAK 6 wg1265 78 fract AAK 6

wg1265 78 fract AAK 14 a

wg1265 88 fract AAA 4

wg1265 89 fract AAC 2 c

wg1265 92 fract AAD 1 c

wg1265 93 fract AAG 3 c

wg1265 89 fract AAC 7 b

Nano-Rheology Nano Rheology by Atomic Force Microscopy

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

Nano-rheology: Theory G ( ) F * 0 2 6 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, 1990-1998. 1998

Stage/Detector Movement for Probe Resting on Glass Plate 4 3 2 1 0-1 -2 0 50 100 150 200 250 300 350 Stage Probe y = 0.805 + 0.0018*t - 2.472 *sine(0.0975*t + 1.8157) - detector y = 0.895-0.235*sine(0.0975*t +1.8153) - stage Time(sec)

y Asin( t ) Stage/Detector Movement for 57 Pa s Viscosity Standard at 25 C 1.6 1.4 Stage(volts) Detector(volts) y = 0.947 + 0.474*sin(9.46*t + 5.888) - stage y = 1.044 + 0.192*sin(9.46*t + 7.489) - detector 1.2 1 0.8 0.6 0.4 10.2 10.4 10.6 10.8 11 11.2 11.4 11.6 time(sec)

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.