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Pressure (kPa) Radius (mm) Pressure x Radius (kN/m) 5.4.4.5.2 Acetoacetate/AA2024-T3 interface CIBT experiments were performed on samples prepared by NAVAIR. A full factorial matrix of cleaning/deoxidizing and CC treatments followed by application of acetoacetate was studied. Figure 4.32 shows the pressure and radius versus time and also Pxr product versus radius for a sample that was not cleaned/deoxidized or pretreated. This behavior is representative of the rest of the samples. The same behavior found previously for primers that adhesively failed during BT was exhibited by these samples. Namely, blister growth started before the maximum pressure, a pressure peak was observed, blister growth kinetics were fast at the beginning of adhesive failure followed by a decrease, and Pxr exhibited a peak, Figure 4.33. All samples delaminated without fracturing except for the NCP samples, which fractured after little delamination. The NCP samples that were not cleaned/deoxidized reached the maximum Pxr value before fracturing, but the cleaned/deoxidized samples did not. Pretreatment improved adhesion strength of acetoacetate to non-cleaned/deoxidized samples in the following order: no CC < TCP < CCC < NCP. The cleaning/deoxidizing step improved adhesion for no CC, NCP, and TCP samples, but it deleteriously affected the CCC samples. Adhesion strength for cleaned/deoxidized samples followed: No CC < CCC < TCP < NCP. The adhesion strength values for each coating system are shown on Figure 4.34. The dotted arrows in the samples cleaned/deoxidized and treated with NCP mean that the adhesion strength of that sample is higher than the value shown. The maximum Pxr could not be measured due to primer rupture, as explained previously. The cleaning/deoxidizing step increased adhesion strength of the samples with no CC by a factor of approximately 2. The same trend was found for the TCP sample although the improvement was not as high as for the no CC samples. No effect of cleaning/deoxidizing on NCP samples was observed. However, the samples cleaned/deoxidized and treated with NCP fractured before the Pressure (bars) no cl no pret acet2 adhesion strength could be assessed. Cleaning/deoxidizing decreased the adhesion strength of Radius (mm) no cl no pret acet2 Pxr no cl no pret acet2 CCC samples, but, in general, cleaning/deoxidizing and CC were found to improve adhesion. Sept 14 2011 88 no cl no pret acet2 3:28:40 PM 10/10/2011 Sept 14 2011 88 no cl no pret acet2 3:28:40 PM 10/10/2011 25 8 0.05 20 7 6 0.04 15 5 0.03 10 5 4 3 2 0.02 0.01 0 1 0 2000 4000 6000 8000 1 10 4 1.2 10 4 Time (s) (a) 0 1 2 3 4 5 6 7 8 Radius (mm) (b) Figure 4.32. BT results related to (a) the behavior of pressure and radius versus time and (b) pressure x radius trend for sample neither cleaned/deoxidized, nor treated, and coated with acetoacetate. 198
Adhesion Strength (J/m 2 ) Pressure x Radius (kN/m) Pressure x Radius (kN/m) PxR no cl no pret acet1 Pxr no cl no pret acet2 Pxr no cl 5200 acet1 Pxr no cl 5200 acet2 Pxr no cl T5900 acet2 Pxr no cl 1200S acet1 Pxr no cl 1200S acet2 Pxr cl no pret acet1 Pxr cl no pret acet2 Pxr cl 5200 acet1 Pxr cl 5200 acet2 Pxr cl T5900 acet1 Pxr cl T5900 acet2 Pxr cl 1200S acet1 Pxr cl 1200S acet2 0.2 Sept 13 2011 88 no cl no pret acet1 Non-cleaned/deoxidized Substrate 0.2 Sept 14 2011 88 cl no pret acet1 Cleaned/Deoxidized Substrate 0.15 NCP 0.15 NCP 0.1 0.1 CCC TCP 0.05 TCP No CC 0 1 2 3 4 5 6 7 8 Radius (mm) (a) 0.05 No CC CCC 0 1 2 3 4 5 6 7 8 Radius (mm) (b) Figure 4.33. Pressure x radius trend for samples (a) non-cleaned/deoxidized and (b) cleaned/deoxidized and coated with acetoacetate. 25 20 15 10 5 0 No C/D No CC No C/D No CC C/D no CC C/D no CC No C/D NCP No C/D NCP C/D NCP C/D NCP No C/D TCP No C/D TCP C/D TCP C/D TCP No C/D CCC No C/D CCC C/D CCC C/D CCC Coating Systems Figure 4.34. Effect of cleaning/deoxidizing and CC on the adhesion strength of acetoacetate to AA2024-T3. C/D means cleaned/deoxidized. 5.4.4.6 Effect of Sample Contamination 280 samples were abraded randomly using 600 grit SiC papers and taken to NAVAIR for treatment and coating application. A full factorial matrix was prepared taking into account cleaning/deoxidizing or no cleaning/deoxidizing and different CC (Section 4.3.3). These samples 199
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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
Page 181 and 182: Scintag (now ThermoARL) Pad-V TM an
Page 183 and 184: Table 3.5. Characterization of bent
Page 185 and 186: Zn 2+ cation release (meq/100g) Pr
Page 187 and 188: (a) (b) (c) Figure 3.33. (a) An exp
Page 189 and 190: |Z| (ohm) Phase angle (degrees) 5.3
Page 191 and 192: |Z| at 0.01 Hz (ohm.cm 2 ) Pore Res
Page 193 and 194: |Z| at 0.01 Hz (ohm.cm 2 ) |Z| at 0
Page 195 and 196: pigmented coatings exhibited partia
Page 197 and 198: 5.3.3.6 Conclusions 1. Exchange ben
Page 199 and 200: 39. M. Mahdavian and M. M. Attar, P
Page 201 and 202: 100. F.Liebau, Structural Chemistry
Page 203 and 204: of the coated sample, which is tigh
Page 205 and 206: Lubricant Blue (Struers) was used f
Page 207 and 208: 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: Pressure (kPa) Pressure (kPa) Radiu
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 and 260: The presence of a salt that has no
Page 261 and 262: This approach yields two figures of
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
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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
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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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