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i (mA/cm 2 ) i (mA/cm 2 ) Replated Cu Figure 7.15. Pit morphologies under polyurethane coatings on as-deposited Al-Cu thin films (left) and aged Al-Cu thin films (right) at different exposure times. (a) 8 (b) 8 7 6 R 2 =0.98 7 6 R 2 =0.97 5 5 4 4 3 3 2 1 i=9.38-9.78 -6 *t 0 0 1x10 5 2x10 5 3x10 5 4x10 5 5x10 5 6x10 5 7x10 5 8x10 5 time s 2 1 0 0.0 2.0x10 5 4.0x10 5 6.0x10 5 8.0x10 5 1.0x10 6 1.2x10 6 1.4x10 6 Time (s) i=a*t -0.92 Figure 7.16. Anodic current densities as a function of time. (a) as-deposited thin film (b) aged thin film. 5.7.5 References 1. L. Balazs et al., Physica A, 217, 319 (1995). 2. G. S. Frankel, Corros. Sci, 30, 1203-1218 (1990). 358
3. L. Balazs, Physica E, 54, 1183-1189 (1996). 4. Y. Hisamatsu et al., Localized Corrosion NACE-3 (ed. R.W. Staehle, B. F. Brown, J. Kruger and A. Agrawal), p.240. 5. D. Lu et al., Corros. Sci, 58, 137-143 (2002). 6. A. J. Griffin Jr. et al., in 30th Annual Proceedings-Reliability Physics 1992, p.239, IEEE/IRPS, New York (1992). 7. S. E. Hernandez et al. J. Electrochem. Soc., 142, 1215-1220(1995) 8. D. R. Frear et al., Metallurgical Transactions, 21A, 2449-2458 (1990). 9. J. Proost et al., J Solid State Electrochem, 2, 150-155 (1998). 10. R. G. Buchheit et al., CORROSION/2001 Research Topical Symposium—Localized Corrosion, (Houston, TX: NACE International, 265-292 (2001). 11. G. S. Frankel et al., J. Electrochem. Soc. 139, 2196-2201 (1992) 359
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FINAL REPORT Scientific Understandi
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This report was prepared under cont
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List of Acronyms AES Atomic Emissio
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List of Figures Figure 1.1. Figure
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Figure 1.21. Figure 1.22. Figure 1.
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Figure 3.11. Cathodic polarization
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Figure 4.12. Average Roughness of R
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Figure 5.4. Figures 5.5. Apparatus
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Figure 5.36. Figure 5.37. R paramet
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Figure 6.23. Two commercial samples
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Figure 7.1. a) instrumental configu
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List of Tables Table 1.1. Table 1.2
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Table 6.4. Processing parameters fo
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Keywords 1. Al alloys 2. Non-chroma
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1. Executive Summary This report su
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the role of electrophoresis in inhi
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occurring at low pHs and release at
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were obtained by a post treatment w
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4. G.O. Ilevbare, J.R. Scully, J. Y
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3. Objective The primary objective
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5. Results and Accomplishments In t
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powder, slurried with ultrapure wat
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TCP-coated AA2024-T3. A Kratos AXIS
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X-ray Photoelectron Spectroscopy (X
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Potential (V vs. Ag/AgCl) -0.2 -0.3
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Signal Intensity (counts/s) assessi
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Al (including both Al 0 and Al 3+ c
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TEM or during sample preparation, s
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Potential (V vs. Ag/AgCl) and uncoa
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5.1.4.8 Effects of Aging on the Fil
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Intensity (counts/s) Concentration
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|Z| 0.01Hz (ohm cm 2 ) |Z| 0.01Hz (
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The artificial scratch cell was als
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Raman intensity, a.u. 4000 880 3500
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Figure 1.24. Raman spectra for the
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peak at 520 cm -1 and an intense Cr
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Figure 1.28. Plots of the intensity
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Figure 1.30. (A) Video micrograph o
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The Zr and O signals arise from the
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Figure 1.35. (A) Corrosion potentia
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Table 1.1. Corrosion current (i cor
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additional pitting. The TCP coating
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Figure 1.41. Cr(VI) peak intensity
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Work is ongoing to understand how t
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9. L. Li, D-Y. Kim and G. M. Swain,
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carefully rinsed with DI water, air
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decrease to a net anodic current in
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Potential (mV vs. SCE) Potential (m
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i (A/cm 2 ) Immediately after silic
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Potential (mV vs. SCE) Rp (ohm.cm 2
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2.4.4 In situ AFM Scratching Result
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Figure 2.31. In situ AFM scratching
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(2.3) Figure 2.35. Specie diagram f
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concentration and the silicon to ca
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analysis coupled with XPS revealed
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5.2.4.4 In Situ AFM Scratching Befo
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esults in the formation of silicate
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26. P. Schmutz and G.S. Frankel, J.
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Pr 3+ , Y 3+ showed [12] an order o
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0.1M NaCl solution with varying con
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8.7 through pH 12.6 due to the lowe
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(b) (c) 99
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immersed in Ce 3+ remained bright w
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S phase and dissolution of Al matri
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Corrosion rate, i corr (A/cm 2 ) 6x
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I L (microA) 600 500 400 300 NC (-8
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than that of chromate[35]. Historic
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coupon was immersed with the polish
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5.3.2.4 Results 5.3.2.4.1 Speciatio
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(c) Figure 3.8. Speciation diagram
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E vs. SCE (V) -0.70 -0.75 -0.80 -0.
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E vs. SCE (V) 1000 rpm E vs. SCE (V
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Chemical quantification showed a me
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(a) (b) Figure 3.15. (a) (top) SEM
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E vs. SCE (V) E vs. SCE (V) E vs. S
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-Z" (ohm) -Z" (ohm) -Z" (ohm) -Z" (
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(Figure 3.8b). However, no effect o
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CPS CPS CPS x 2 14 10 12 10 8 6 4 2
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CPS CPS 100 95 90 85 80 75 70 x 10
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I k L 0. 2 1 2 AnFC B D 2 3 O 1
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i -800 (A/cm 2 ) 10 -4 NaCl NaCl+5
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Corrosion rate ( 1/R p ) ohm -1 cm
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particles compared to zinc-free sol
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and Zn bentonite compounds have red
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2) Deoxidizing for 3 minutes in an
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Scintag (now ThermoARL) Pad-V TM an
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Table 3.5. Characterization of bent
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Zn 2+ cation release (meq/100g) Pr
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(a) (b) (c) Figure 3.33. (a) An exp
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|Z| (ohm) Phase angle (degrees) 5.3
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|Z| at 0.01 Hz (ohm.cm 2 ) Pore Res
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|Z| at 0.01 Hz (ohm.cm 2 ) |Z| at 0
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pigmented coatings exhibited partia
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5.3.3.6 Conclusions 1. Exchange ben
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39. M. Mahdavian and M. M. Attar, P
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100. F.Liebau, Structural Chemistry
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of the coated sample, which is tigh
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Lubricant Blue (Struers) was used f
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good grip on the dolly, the equipme
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Pressure (kPa) r (mm) Pressure x Ra
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Pressure x Radius (kN/m) plateau bu
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Pressure x Radius (kN/m) Pxr (KN/m)
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Average Roughness (m) In contrast,
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Adhesion Strength (J/m 2 ) PVB PVB
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Pressure (kPa) Constant Infusion up
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(a) (b) (c) (d) Figure 4.19. Coatin
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Min. Potential (V vs SHE) Min. Pote
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Pressure (kPa) exposure in hot wate
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Engineering Stress (MPa) slope of t
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Adhesion Strength (J/m 2 ) ASTM D33
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Pressure (kPa) Pressure (kPa) Radiu
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Adhesion Strength (J/m 2 ) Pressure
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Table 4.7. Adhesion Strength values
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Non-Cl./Deox. No CC Cleaned/Deox. N
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5.4.5 Conclusions and Implications
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5.5 Task 5: Inhibitor Activation an
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solution for equilibration at contr
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Table 5.2. Techniques applied to sp
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The capacitance was determined by E
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combination with zinc molybdate, a
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Concentration, mmol / L Final pH te
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Alkaline affects praseodymium solub
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MoO 4 2- ) inhibition to the system
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Zinc molybdate is reported to be si
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The presence of a salt that has no
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This approach yields two figures of
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Inhibitor mapping of the Hentzen 16
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The molybdate loss in the strontium
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The capacitance dC is given by 0 (
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2 C( r, t) C( r )[1 r 2 exp( D nt
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-thea (degree) logIZI (Ohm-Cm 2 ) P
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Capacitance (F) respectively. The c
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Capacitance (F) Weight gain (g) For
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Normalized Capacitance Change Norma
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Potential V (Ag/AgCl) Corrosion rat
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5.5.4.7 Nanopore structure characte
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Normaalized Transport Rate (g/m^2_d
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S-Parameter S-Parameter Penetration
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S-Parameter S-Parameter Penetration
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R-parameter R-parameter Penetration
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5. T. M. Letcher, “Thermodynamics
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pigment of CaSiO 3 with initial pH
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allowed a comparison of the differe
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The solution resistance (R sol ) va
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Theta [degrees] theta |Z| [ohm] 10
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C [F/cm2] Rcorr [ohm*cm2] 7075-AHN
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C [F/cm 2 ] Rcorr [ohm*cm 2 ] Rcorr
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Visual TTF [hours] Table 6.2. Param
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of Metallast pre-treatment, which h
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Prediction of the TTF obtained by A
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5.6.2 Electrochemical Impedance Spe
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5.6.2.2.1 Coating system descriptio
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Table 6.4. Processing parameters fo
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population of total TTF vectors th
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components of the impedance and the
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Figure 6.17. EIS spectra for sample
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Figure 6.18. Kaplan-Meier survival
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Maximum c i range Maximum ci range
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The type and number of input neuron
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Predicted TTF The BFM method, intro
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The most significant variables to i
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5.6.3 Characterization of Pigment D
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of sputtering gold and carbon paint
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Figure 6.26. Cross-sectional view o
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Figure 6.28. EDX maps of primer cro
Page 341 and 342: Figure 6.31. EDX maps of primer cro
Page 343 and 344: In Figure 6.34, Ca and Si existed a
Page 345 and 346: Table 6.8. Average percentage resid
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Page 349 and 350: Figure 6.37. Coating systems in det
Page 351 and 352: Each corrosion volume of scribed ar
Page 353 and 354: Corrosion Area (mm 2 ) 1200 1000 80
Page 355 and 356: Corrosion Area (mm 2 ) Corrosion Ra
Page 357 and 358: Corrosion Rate (mm/yr) Corrosion Vo
Page 359 and 360: Corrosion Area (mm 2 ) corrosion ra
Page 361 and 362: corrosion rate (mm/yr) Corrosion Vo
Page 363 and 364: Corrosion Volume (mm/yr) Corrosion
Page 365 and 366: ate, PPG CA7233 coated samples had
Page 367 and 368: Appendix 6B Table 6B.1. Corrosion v
Page 369 and 370: Table 6B.3. Corrosion rate of sampl
Page 371 and 372: Table 6B.5. Corrosion area of sampl
Page 373 and 374: 5.7. Task 7: Characterization of Lo
Page 375 and 376: at 65C. After using DI water to rin
Page 377 and 378: Transmission Mode Conduct EIS measu
Page 379 and 380: Cdl(F/cm 2 ) Rp(.cm 2 ) relatively
Page 381 and 382: pit bottom area (cm 2 ) pit bottom
Page 383 and 384: 2days 2days 1mm 1mm 7days 7days Pit
Page 385 and 386: (a) (b) Si Si O Al Na Ca K Si Al-Cu
Page 387 and 388: Pit 1 and pit 2 as shown in Figure
Page 389 and 390: In these experiments, Deft primers
Page 391: For the case of as-deposited thin f
Page 395 and 396: and subsequently re-oxidized in two
Page 397 and 398: not represent true adhesion strengt
Page 399 and 400: • The pit morphology in 0.5 M NaC
Page 401 and 402: Appendix 2. List of Scientific/Tech
Page 403 and 404: “The Secret Life of Chromate Free
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