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Post-spray Pre-spray Figure 5.11. Pr speciation in the presence of calcium sulfate (OLI Stream Analyzer). Salt Spray Exposure Effect on CaSO 4 and Pr(OH) 3 Pigments Primer sample on 20424- T3 Al with Alodine 600 chromate conversion coating EDX Maps Pr O Ca S Al Sharp image; Ca-O-S match well; sharp Al-coating interface. [Pr] in Pr poor region = 4.2 wt% +/- 3.8% Pr O Ca S Al Image lose contrast; Pr-Ca-S match well; diffused Al-coating interface. [Pr] in Pr poor region = 11.4 wt% +/- 1.4% 3 Figure 5.12. EDXS Inhibitor Mapping of Deft 44GN098 primer before (above) and after (below) 2000-hour ASTM B117 salt spray test. Statistical techniques were applied to the data in the inhibitor field maps to reveal and quantify spatial and chemical distribution trends. The approach taken, as shown in Figure 5.13, is to isolate horizontal (in the primer plane) and vertical (through the primer plane) line scans from the maps, and to apply correlation analysis to the element pairs within each line scan. 226
This approach yields two figures of merit for each element pair in each line scan: the Pearson product moment (r 2 ) is a robust measure of the variation in the concentrations of the element pairs that can be attributed to linear covariation, with the regression slope for each element pair as a second measure of covariance with greater sensitivity but potentially lower confidence. These figures of merit can be used to compare inhibitor distributions in primer films as a function of either exposure history or distance from the substrate or air-interface of the primer film. Figure 5.13. Statistical treatment of inhibitor spatial maps. Figure 5.14 shows the results of applying the higher confidence figure of merit, r 2 , to describe correlation in the pairs of elements shown in spatial map of the Deft GN44098 primer shown in Figure 5.13. The y-axis of this Figure shows the change in the r 2 parameter produced by the salt spray test as measured in the sets of horizontal and vertical line scans. This analysis shows the positive correlation of praseodymium with the carbon of the primer matrix produced by the salt spray test, the strong de-correlation of calcium with sulfur, and the drop in correlation of both calcium and sulfur with the carbon matrix following the salt spray test. This is interpreted as the mobilization of praseodymium through the primer matrix, the dissolution of parent CaSO 4 pigment particles, and an overall loss of both calcium and sulfur in the primer matrix produced by the salt spray test. Analyzing the data of Figure 5.13 by the regression slopes of element pairs reveals additional interactions, as shown in Figure 5.15. In this Figure, the y-axis is the change in slope of the element pair regression lines produced by the 2000-hour salt spray test. This treatment reveals a proportional covariation developing between praseodymium and both sulfur and calcium as a consequence of the salt spray test. This is explainable by the formation of praseodymium sulfate 227
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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
Page 209 and 210: Pressure (kPa) r (mm) Pressure x Ra
Page 211 and 212: Pressure x Radius (kN/m) plateau bu
Page 213 and 214: Pressure x Radius (kN/m) Pxr (KN/m)
Page 215 and 216: Average Roughness (m) In contrast,
Page 217 and 218: Adhesion Strength (J/m 2 ) PVB PVB
Page 219 and 220: Pressure (kPa) Constant Infusion up
Page 221 and 222: (a) (b) (c) (d) Figure 4.19. Coatin
Page 223 and 224: Min. Potential (V vs SHE) Min. Pote
Page 225 and 226: Pressure (kPa) exposure in hot wate
Page 227 and 228: Engineering Stress (MPa) slope of t
Page 229 and 230: Adhesion Strength (J/m 2 ) ASTM D33
Page 231 and 232: Pressure (kPa) Pressure (kPa) Radiu
Page 233 and 234: Adhesion Strength (J/m 2 ) Pressure
Page 235 and 236: Table 4.7. Adhesion Strength values
Page 237 and 238: Non-Cl./Deox. No CC Cleaned/Deox. N
Page 239 and 240: 5.4.5 Conclusions and Implications
Page 241 and 242: 5.5 Task 5: Inhibitor Activation an
Page 243 and 244: solution for equilibration at contr
Page 245 and 246: Table 5.2. Techniques applied to sp
Page 247 and 248: The capacitance was determined by E
Page 249 and 250: combination with zinc molybdate, a
Page 251 and 252: Concentration, mmol / L Final pH te
Page 253 and 254: Alkaline affects praseodymium solub
Page 255 and 256: MoO 4 2- ) inhibition to the system
Page 257 and 258: Zinc molybdate is reported to be si
Page 259: The presence of a salt that has no
Page 263 and 264: Inhibitor mapping of the Hentzen 16
Page 265 and 266: The molybdate loss in the strontium
Page 267 and 268: The capacitance dC is given by 0 (
Page 269 and 270: 2 C( r, t) C( r )[1 r 2 exp( D nt
Page 271 and 272: -thea (degree) logIZI (Ohm-Cm 2 ) P
Page 273 and 274: Capacitance (F) respectively. The c
Page 275 and 276: Capacitance (F) Weight gain (g) For
Page 277 and 278: Normalized Capacitance Change Norma
Page 279 and 280: Potential V (Ag/AgCl) Corrosion rat
Page 281 and 282: 5.5.4.7 Nanopore structure characte
Page 283 and 284: Normaalized Transport Rate (g/m^2_d
Page 285 and 286: S-Parameter S-Parameter Penetration
Page 287 and 288: S-Parameter S-Parameter Penetration
Page 289 and 290: R-parameter R-parameter Penetration
Page 291 and 292: 5. T. M. Letcher, “Thermodynamics
Page 293 and 294: pigment of CaSiO 3 with initial pH
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Page 297 and 298: The solution resistance (R sol ) va
Page 299 and 300: Theta [degrees] theta |Z| [ohm] 10
Page 301 and 302: C [F/cm2] Rcorr [ohm*cm2] 7075-AHN
Page 303 and 304: C [F/cm 2 ] Rcorr [ohm*cm 2 ] Rcorr
Page 305 and 306: Visual TTF [hours] Table 6.2. Param
Page 307 and 308: of Metallast pre-treatment, which h
Page 309 and 310: 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
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Figure 6.31. EDX maps of primer cro
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In Figure 6.34, Ca and Si existed a
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Table 6.8. Average percentage resid
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strictly limited due to the barrier
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Figure 6.37. Coating systems in det
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Each corrosion volume of scribed ar
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Corrosion Area (mm 2 ) 1200 1000 80
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Corrosion Area (mm 2 ) Corrosion Ra
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Corrosion Rate (mm/yr) Corrosion Vo
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Corrosion Area (mm 2 ) corrosion ra
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corrosion rate (mm/yr) Corrosion Vo
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Corrosion Volume (mm/yr) Corrosion
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ate, PPG CA7233 coated samples had
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Appendix 6B Table 6B.1. Corrosion v
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Table 6B.3. Corrosion rate of sampl
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Table 6B.5. Corrosion area of sampl
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5.7. Task 7: Characterization of Lo
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at 65C. After using DI water to rin
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Transmission Mode Conduct EIS measu
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Cdl(F/cm 2 ) Rp(.cm 2 ) relatively
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pit bottom area (cm 2 ) pit bottom
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2days 2days 1mm 1mm 7days 7days Pit
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(a) (b) Si Si O Al Na Ca K Si Al-Cu
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Pit 1 and pit 2 as shown in Figure
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In these experiments, Deft primers
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For the case of as-deposited thin f
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3. L. Balazs, Physica E, 54, 1183-1
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and subsequently re-oxidized in two
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not represent true adhesion strengt
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• The pit morphology in 0.5 M NaC
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Appendix 2. List of Scientific/Tech
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“The Secret Life of Chromate Free
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