stress corrosion crack initiation & growth measurements in ...final report prepared under...

MOL.20061109.0070

Report Number: GE-GRC-Bechtel-2006-2

4,0 tk ‘061

Stress Corrosion Crack Initiation & Growth

Measurements in Environments Relevant to

High Level Nuclear Waste Packages

QA

Peter L. Andresen and Young J. Kim

GE Global Research Center

October 2, 2006

Final Report Prepared under Bechtel Purchase Order QA-HC4-00196 by General Electric Global Research Center

Work performed in accordance with purchase order requirements and the

General Electric Global Research Center Quality Assurance

Program for the Corrosion Program, Rev. 1.2, March 12, 2003

GE Final Report October 2, 2006


Final Report for 2Q2006 — Purchase Order QA-HC4-00196

by General Electric Global Research Center

Work performed in accordance with purchase order requirements and the General Electric Global Research Center Quality Assurance

Program for the Corrosion Program, Rev. 1.2, March 12, 2003

"Stress Corrosion Crack Initiation & Growth Measurements in

Environments Relevant to High Level Nuclear Waste Packages"

Final Report on SCC Results — October 2, 2006

Peter Andresen and Young J Kim — GE Global Research Center

This is a final report on the testing on stress corrosion cracking and corrosion — passive film characterization being performed at GE Global Research. Several categories of tests are being performed:

1. SCC growth rate testing in an SCW solution at 150 °C.

2. SCC crack initiation, U-bend testing in an SCW solution at 165 °C.

3. SCC crack initiation, Keno constant load testing in a 15% BSW solution at 105 °C.

4. SCC initiation of air fatigue precracked 0.5TCT specimens at 105 °C. 5. Tensile and creep testing in air of titanium grade 7.

6. Film characterization and corrosion behavior of Ti alloys in salt environments

A detailed description of the experimental techniques, solution chemistries, materials and prior results is given in Reference [1].

1 — SCC growth rate testing, now in an SCW solution at 150 °C.

Three autoclave systems are being used to measure growth rates in CT specimens. The test procedures represent state-of-the-art techniques as described in Reference [1]. The heat and heat treatments for each specimen are shown in Table 1. The specimen pairings were:

• c287/c288 — Ti Grades 29 and 28 (as-received) tested at 27.5 MPa .qm

• c263/c264 — alloy 22, both as-welded and tested at 40 MPa4m

• c265/c266 — alloy 22, as-welded +TCP or + LRO treatment at 40 MPagm

Both Ti Grade 28 and 29 exhibited moderately high growth rates (Figures 1 — 7), although initially Ti Grade 28 started cracking more readily and therefore tended to dominate the early part of the testing (once one specimen begins growing, either its K increases or — with load shedding — the K decreases on the other specimen; either way, one specimen tends to stay dominant). Table 3 tabulates the crack growth data for the Ti Grade 29 and 28 specimens.

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An effort was made to determine the K dependence of Ti Grades 28 and 29 (Figures 8 and 9) by identifying the growth rates during decreasing K (—d1Cda) testing (Figures 3 and 7). However, only limited testing has been performed on the effect of stress intensity factor (K) on crack growth rate behavior of these high strength Ti alloys, and this should be viewed as a preliminary evaluation, not one that establishes the K dependence with confidence.

The most useful data come from specimen c288 of Ti Grade 28 (Figure 7) where a controlled change in K was made using —dK/da, where K changes only in proportion to crack advance so that the material and plastic zone can adjust to the change. These data were re-evaluated over 100 hour increments, and the growth rate vs. K plotted (Figure 8). By using larger increments, more "smoothing" would have been obtained. Overlaid on Figure 8 is the effect of specific K dependencies — i.e., K3 , K4 and le, all anchored to a specific observed point (34.6 MPaqm).

A relatively high K dependence (e.g., K 4 or K6) appears to be a good fit to the data. The evaluation of the much lower crack growth rate data obtained at the same time on c287 (Figure 3) was also done (Figure 9). Because Ti Grades 28 and 29 are not that fundamentally different, and especially because subsequent evaluation of Ti Grade 29 revealed much higher growth rates, it is hard to have much confidence in these data — where the rates are perhaps 50X slower. The data (Figure 9) also shows about a K4 dependence.

This K dependence is higher than observed in higher temperature water, e.g., 288 — 340 °C boiling or pressurized water reactor conditions, where K dependencies in the range of K 15 to K2 • 5 are typical (Figure 10— 12). But these studies have explicitly compared constant K testing (Figure 10) at different K values vs. —dK/da testing (Figure 11) at the same value as used in Figures 8 and 9. Clarification of the effects of K requires both detailed —d1C/da studies over a wider range in K, as well as complementary step-wise evaluation of K employing fatigue cracking to increase or decrease K followed by transitioning to constant K conditions.

All alloy 22 specimens listed in Table 2 were used to study crack growth in the weld metal (Figures 13 — 18), and all exhibited very low growth rates despite the change to a more aggressive environment and a higher temperature (150 —200 °C) compared to earlier tests which were run in 110 °C BSW. They were transitioned very slowly toward longer hold times, but it appears that no sustained growth at constant load is observed. The higher temperature (200 °C) portions of tests c263, c264, c268 and c269 showed negative crack growth, and this most likely results from small amounts of H2 near the deaerated crack tip that forms from corrosion processes causing Ni-metal stability, which creates a shorting path in the wake of the crack [2,3]. This is a transient phenomenon (that is, the crack doesn't forever appear to shorten), but at 200 °C, it could continue for hundreds or thousands of hours. After these specimens were dropped to 175 °C, they exhibit zero crack advance, but the kinetics of "crack shortening" might still affect the data at this temperature. After dropping back to 150C, the data are noisier and less reliable and therefore, in general, are not cited in Table 2 even though the apparent CGRs are lower. Unless transient (< 100 hrs), the higher growth rates tend to be the most credible [4,5]. The recent higher growth rate observation shown in Figure 16 may seem surprising, but the test has been cycling at 40 MPaqm, R=0.7 and 0.001 Hz, and data obtained early in the test under these same conditions showed a growth rate of 7 x 10-8 nun/s, and at 7500 hours a rate of 2 x 10 -8 mm/s. This variation in rate is periodically observed in other cases of environmental cracking at high load ratio, and can be



attributed to crack closure effects from the mismatch in the fracture surface and build-up of oxides (or in this case, silicates) in the crack. The companion (tandem) specimen (c266) shows no such increase, and the test was recently changed to a 9000s hold at Kmax•

2 — SCC crack initiation, U-bend testing in an SCW solution at 165 °C.

These tests have continued, from their initial start in October 2003. The test procedures meet or exceed standards for U-bend testing, as described in Reference [1]. A range of heat treatments and creviced vs. uncreviced U-bends have been exposed. An inspection just occurred at 18,034 hours, and showed no evidence of crack initiation. However, there was an increasing incidence of fine pits on the outer (uncreviced) arm of the double U-bend (Figure 19 and 20), as well as crevice corrosion in a creviced section of one double U-bend. A set of four titanium grade 29 U-bend specimens was added to the test following the 14,056 hours shutdown; this necessitated removal of two of the alloy 22 single U-bend specimens. The current total Alloy 22 specimen exposure time is 17,241 hours and the four titanium grade 29 U-bends have been exposed for 3185 hours. A summary of the Alloy 22 and titanium grade 29 specimens, heat treatments and times-in-test is given in Tables 4, 5, 6. A compilation of Alloy 22 double U-bend outer surface pit size distribution for specimens DUB1189 and DUB1182 is given in Table 7.

3 — SCC crack initiation, Keno constant load testing in a 15% BSW solution at 105 °C.

These tests have continued, although there have been two forced outages (in October 2004 and February 2005) because the leak rate was too high. The test procedures represent state-of-the-art techniques as described in Reference [1]. This results from corrosion of the stainless steels parts used in the Keno system. The system was down for an extended period for the move of the laboratory and to remove the modules manifolds and installed the specimens into more corrosion resistant parts. The test was re-started in early June 2006 and has 28,115 hours (for some specimens) as of October 2, 2006; the new Ti Grades 7 and 29 specimens have 2784 hours exposure. Updated plots of the Keno results are provided (Figures 21 —23), and a listing of the specimens recently removed and new specimens added is given in Table 8.

4 — SCC initiation of fatigue precracked 0.5TCT specimens 15% BSW solution at 114 °C.

Eighteen 0.5T CT specimens were fatigue precracked in air and assembled in three groups in an autoclave and exposed to 15% BSW solution at 105 °C (Table 9). The test procedures represent state-of-the-art techniques as described in Reference [1]. The accumulated time on test is 2928 hours. The specimens will be periodically interrupted and evaluated for crack advance by dc potential drop.

5 — Tensile and creep testing in air of titanium grade 7.

This effort is designed to develop air controls for the Ti Grade 7 keno specimens that were tested in 105C BSW, and secondarily to determine the creep effects in CT specimens. The control tests are being performed in response to concerns for creep failure of Ti Grade 7 (vs. SCC failure). To develop these control data, a combination of tensile tests and creep tests were conducted in 105 °C laboratory air (e.g., see Reference 1, Figures 6-3 through 6-6). The test procedures represent state-of-the-art techniques as described in Reference [1]. The creep data is particularly important, as it shows that the failures obtained in 105 °C "ground water" solutions are likely to have been



predominantly creep failures, and not SCC failures. Creep tests have been performed on round tensile specimens in an autoclave with 105 °C air, and will include new test data on Ti Grades 7 and 29. The specimens were slowly loaded and then maintained at a fixed load while the elongation (displacement) is monitored. The creep data obtained to date simply used the machine actuator (position reading), which works well for materials that readily creep such as Ti Grade 7, but for more creep resistant materials (like Ti Grade 29), extensometer measurement on the specimen surface are needed. We have acquired a "high temperature" (175 —200 °C) extensometer with excellent resolution and stability for use with Ti Grade 29 and similar materials.

Recent creep data on Ti Grade 7 are shown in Figures 24 — 29. Figure 24 shows the response of the actuator position vs. the extensometer; as expected, during loading, some displacement is "absorbed" by the machine and linkage, so the strain applied to the specimen is perhaps two-thirds of the actuator displacement. On initial loading (Figure 25), the yield strength was about 42.5 ksi (293 MPa). The test was held for a few minutes while the yield strength was calculated, then slowly decreased by — 30%, then increased at the same displacement rate. The resulting stress-strain response is shown in Figure 26, which clearly shows a yield point at about 38 ksi (262 MPa). The initial measurement (42.5 ksi) was used as the basis for testing at 111% of yield — i.e., 47.25 ksi (326 MPa). The resulting creep response is shown in Figure 27, with failure in 1.17 hours. It's clear that the orientation and/or the variation in measured yield strength is very important in determining creep life. Based on our prior data, 1.17 hours is a very short creep life for 111% of yield strength, although based on the second yield strength measurement (38 ksi, 262 MPa), the test was done at 124% of yield. It seems appropriate to have used the 262 MPa (38 ksi) yield stress as the basis for interpreting this test.

A follow-on test was done using a perpendicular orientation from the plate of Ti Grade 7. The yield strength was measured during initial loading (Figure 28), where again there was some difference between actuator displacement and extensometer strain. The yield strength was measured at 36 ksi (248 MPa), and the specimen was then loaded to 114.7% of yield strength (41.3 ksi, 285 MPa). Figure 29 shows the creep response, with failure at 143.06 hours.

6— Film Characterization and Corrosion Behavior of Ti Alloys in Salt Environments.

Overview and Background

The corrosion behavior of various Ti alloys has been studied at 120 °C or 150 °C in mixed salt environments. Measurements of open-circuit potential (OCP) versus time, electrochemical impedance (El) and cyclic potentiodynamic polarization (CPP) behavior were conducted to evaluate the passivity of these alloys and to calculate the corrosion rate.

This program is designed to examine the corrosion characteristics and passive film properties of the drip shield Ti alloys to increase understanding of the expected SCC and hydrogen induced cracking (HIC) response under repository relevant conditions. The drip shield is an essential element of the engineered barrier system, and the ability to provide very long waste package lifetimes that can be predicted with confidence is a central factor in the calculated release rate of radionucleides from the mountain.



Experimental Procedures

Chemical compositions of various Ti alloys (Ti Grade 7, Ti Grade 23+Pd, Ti Grade 29, AKOT) tested in this study are shown in Table 10. Chemical compositions of Ti Grade 7, Ti Grade 23+Pd, and Ti Grade 29 were verified by Laboratory Testing, and that of AKOT alloy (being tested as a comparison alloy) was provided by Kobe Steel Company.

The specimens used for electrochemical testing were cut by electrodischarge machining in the form of 1/8" x 1/8" x 2" (Ti Grade 29), 1/8" x 1/16" x 2" (Ti Grade 23+Pd), 1/8" diameter x 2" long (Ti Grade 7), and 1/8" x 1/32" x 2" (AKOT Kobe steel); the specimens for hydrogen uptake measurements were 3/8" x 3/8" x 1/32" for all alloys. All specimens were wet-polished to a 600 grit paper. Two different surface treatments were done before the testing; (1) polished fresh surface and (2) preoxidized surface at 400 °C for 24 hours in air. Specimens for electrochemical measurements were spot welded to a polytetrafluoroethylene (PTFE)-insulated Ti wire and mounted in a Conax fitting. After immersion of three coupons of each alloy in the test solutions, the hydrogen content was measured by LTI. The test procedures represent state-of-the-art techniques as described in Reference [1].

The chemicals used for the test chemistry is shown in Table 11. All test solutions were prepared from reagent grades in high purity water. The chemicals were mixed with water that had been heated to the boiling point in the autoclave. All testing was performed in a commercial-purity titanium autoclave. To prevent evaporative loss of water, a six foot long tube-in-tube heat exchanger was used, with cooling water on the outside. The solution level in the test autoclave was monitored periodically by checking for continuity between the autoclave and an insulated Ti wire feed-through bar. No water addition was needed. In addition, air or Ar at 100 psi was continuously purged in the test autoclave in order to maintain constant pressure above the solution.

All potentials were measured with respect to an internal 0.1N KC1 Ag/AgCl. A platinum flag electrode was also employed. ECP values were measured at the test temperature; they were not corrected to room temperature. All tests were performed at 120 °C or 150 °C ± 1 °C. CPP scans at 0.17 mV/second were started at 50 mV below the steady-state corrosion potential obtained 1 hour after immersion in solution and reversed when a current density of 5 mA/cm 2 or an applied potential of 1.0V vs. reference electrode was reached.

Experimental measurements were performed in regular sequence as followed: (1) OCP measurement for 4 weeks in aerated solution, (2) Polarization resistance measurement by EIS in aerated solution, (3) OCP measurement for 1 week in deaerated solution by purging Ar, and (4) CPP measurement in deaerated solution by purging Ar.

Results and Discussion

Open-Circuit Potential Behavior

OCP measurements were performed to evaluate the oxide stability and corrosion resistance of the Ti alloys. OCP behaviors of the Ti alloys in TS-1, TS-2, TS-3, and TS-4 are shown in Figures 30 — 33. OCP of all test electrodes was similar, being stable with time. Once the solution was deaerated by



purging Ar gas, the OCP decreased with time. Among four different test environments, slightly higher OCP was measured only in aerated TS-1 solution, while under deaerated condition, OCPs of the Ti alloys are very similar; decreasing with time. Under the mixed-salt solution the passive films on the Ti alloys would be expected to become so protective and stable that contributions from metal corrosion should become extremely small, and redox reactions from the species in solution should be stable. During the OCP measurement in aerated condition, the oxygen reduction reaction predominantly controlled the OCP and thus the OCP in aerated solution is higher than one in deaerated solution.

Polarization Resistance by El

The electrochemical impedance (El) measurement technique is being used to investigate the corrosion behavior of materials in conducting and non-conducting media. Electrochemical impedance measurements provide a variety of electrochemical kinetics data such as polarization resistance, coating resistance, diffusion kinetics, capacity, etc.

Despite EIS has been used as a very useful method for the analysis of corrosion processes with many fundamental advantages over other electrochemical techniques, researchers find the complexity of the data analysis for a given system where the transfer function should be driven from the kinetics of the partial reactions involved in the corrosion process. The time required to obtain a full impedance diagram imposes a serious limitation to the technique when the test specimens reacts relatively rapidly or slowly. Furthermore, the rate of mass transfer to the corroding interface can control the oxide/hydroxide corrosion product that results in the EIS analysis.

Figures 34 —45 show the impedance spectra for Ti alloys at the open-circuit potential in TS-1, TS-2, TS-3, and TS-4. The Bode plots of the Ti alloys are shown in Figures 34— 37, and the Nyquist plots in Figures 38— 41. The phase angles of the Ti alloys are shown in Figures 42 — 45. The impedance magnitude spectra for Ti alloys tested in four different test environments show a similar polarization resistance. However, as seen in Figure 42, spectra for Ti Grade 7 and AKOT tested in TS-1 and Figure 44 in TS-3 had two relaxation time constants after immersion, indicating possible two oxide layer that can be explained by the formation of additional oxide layer or transformation of one oxide to another, while such a typical phase angle was not observed on the same alloys tested in TS-2 and TS-4. However, no surface analysis was performed to identify the oxide structure.

Cyclic Potentiodynamic Polarization

The CPP measurement was conducted to detect any breakdown of passivity, such as pit and crevice initiation potentials and repassivation potential if losses in passivity were observed. Figures 46 — 53 show the CPP behavior of the Ti alloys, fresh (non-oxidized) or preoxidized surface, in four different salt solutions. Ti alloys tested in salt solutions showed the similar polarization behavior, and no localized corrosion attack on the sample surface was observed after the CPP measurement. This CPP curve shows that the Ti alloys maintain its passivity at potentials at least as high as 500 mV (vs. Ag/AgC1).



Hydrogen Content

The characteristics of oxide films have considerable influence on both the corrosion resistance and the hydrogen absorption by the metal. The porosity, electric conductivity, or permeability of the oxide to protons will control how much hydrogen from the corrosion reaction enters the metal. Table 12 shows the hydrogen take-up by different Ti alloys before and after immersion in the test solutions in the mixed-salt solution (TS-1, TS-2, TS-3, and TS-4) at 120 °C or 150 °C. The data value represents the average value of three specimens of each test alloy and shows no significant hydrogen take-up by these alloys during the short immersion time. It may require a longer immersion time to allow more hydrogen take-up.

Calculation of Corrosion Rate

The corrosion rate of the Ti alloys was calculated by using the polarization resistance, weight loss, corrosion current density from CPP. All techniques are described in ASTM G 1, ASTM G 59, and ASTM G 102. Table 13 shows the corrosion rate of the Ti alloys in the test solutions in the mixed-salt solution (TS-1, TS-2, TS-3, and TS-4) at 120 °C or 150 °C. Three different methods were used to calculate the corrosion rate.

All test alloys show the similar corrosion rate in these test solutions. It is seen that the corrosion rate calculated by the corrosion current density from the CPP curve and the weight loss measurement are in good agreement, while the corrosion rate by EIS is higher. The high corrosion rate calculated by EIS may be caused by the polarization resistance measurement within limited frequency ranges that is explained by incomplete semi-circle behavior of Nyquist plots shown in Figures 38 —41. Also, as stated above, the partial redox reactions on the surface/solution interface may also contribute the high corrosion rate. In general, the corrosion rate calculated by the weight loss measurement provides more accurate estimation.

Conclusions

The passivity of the Ti alloys was examined by measuring the open-circuit potential and polarization behavior in the mixed-salt environment at 120 °C or 150 °C. Steady-state corrosion potentials of the Ti alloys were measured, and no evidence of localized corrosion attack on all alloys after polarization measurements was observed. Also, there was no significant hydrogen take-up by the Ti alloys after the free immersion in the test solutions.



References:

[1] — P.L. Andresen, Y.J. Kim, P.W. Emigh, G.M. Catlin and P.J. Martiniano, "Stress Corrosion Crack Initiation & Growth Measurements in Environments Relevant to High Level Nuclear Waste Packages", Report # GE-GRC-Bechtel-2005-1, Final Report to Bechtel Corp. for FY2005 Prepared under Purchase Order QA-HC4-00196, December 9, 2005.

[2] — P.L. Andresen, P.W. Emigh, M.M. Mona and J. Hickling, "Effects of PWR Primary Water Chemistry and Deaerated Water on SCC", Proc. 12 th Int. Symp. on Environmental Degradation of Materials in Nuclear Power Systems — Water Reactors", TMS, Snowbird, August 2005.

[3] — S.A. Attanasio and D.S. Morton, "Measurement of the Ni/Ni0 Transition in Ni-Cr-Fe Alloys and Updated Data and Correlation to Quantify the Effect of Aqueous Hydrogen on Primary Water SCC", Proc. 11 th Int. Symp. on Environmental Degradation of Materials in Nuclear Power Systems, ANS, 2003.

[4] — P.L. Andresen, "SCC Testing and Data Quality Consideration", Proc. Ninth Int. Symp. on Environmental Degradation of Materials in Nuclear Power Systems - Water Reactors, AIME, 1999.

[5] — P.L. Andresen, "Perspective and Direction of Stress Corrosion Cracking in Hot Water", Proc. 10th Int. Symp. on Environmental Degradation of Materials in Nuclear Power Systems - Water Reactors, NACE, 2001.



Table 1 — CT Specimen Heats and Heat Treatments

The crack plane in all of these CT specimens is in the weld metal

Specimen ID Material — Heat Heat Treatment ' Stress Intensity Factor

C263 C22 — 2277-0-3183 As-welded 40 MPaqm

C264 C22 — 2277-0-3183 As-welded 40 MPaqm

C265 C22 —2277-0-3183 As-welded+TCP 40 MPaqm

C266 C22 —2277-0-3183 As-welded+LRO 40 MPaqm

C287 Ti Gr.29 — 956205 As-received 27.5 MPaqm

C288 Ti Gr.28 — 870749601 As-received 27.5 MPa4m

TCP = 650°C for 200 hours LRO = 550°C for 10 hours



Table 2a — Crack Growth Rates for Welded Alloy 22 CT Specimens Data in SCW chemistry; Crack growth in the weld metal; AW=As-welded

Specimens c268 and c269 are no longer in test, but are reported here for completeness

Unless transient (< 100 hrs), the higher growth rates are the most credible (Ref [4,5])

Specimen TD Temp., Heat Loading, CGR, (K)

Figure* °C Treatment R/v/hold** mm/s

C263 (40 MPa\lm) 1-73 150 AW 0.7, 0.001 Hz 2.1 --> 0.5 x 10-8 -

C263 (40 MPa4m) 1-73 150 AW 0.6, 0.001 Hz 1.1 x 104

C263 (40 MPaqm) 1-73 150 AW 0.7, 0.001 Hz, 3000s 3 x le -

C263 (40 MPa4m) 1-74 150 AW 0.7, 0.001 Hz, 9,000s 1.2 x 10-9

C263 (40 MPa\lm) 1-74 150 AW 0.7, 0.001 Hz, 85,400s 1.2 x le

C263 (40 MPa4m) 1-75 200 AW 0.7, 0.001 Hz, 3000s Note (1)

C263 (40 MPaqm) 1-75 175 AW 0.7, 0.001 Hz, 85,400s . 0 Note (2)

C263 (40 MPa4m) 7, 1-76 150 AW 0.7, 0.001 Hz, 85,400s .... 0 Note (3)

C264 (40 MPa4m) 1-81 150 AW 0.7, 0.001 Hz 20 --> < 1 x 10-9

C264 (40 MPaqm) 1-81 150 AW 0.6, 0.001 Hz 2 x 10-9

C264 (40 MPa4m) 1-82 150 AW 0.7, 0.001 Hz, 3000s 1.3 x 10-9

C264 (40 MPaNim) 1-82 150 AW 0.7, 0.001 Hz, 9000s 1.3 x 10-9

C264 (40 MPa4m) 1-82 150 AW 0.7,0.001 Hz, 85,400s---- 0

C264 (40 MPa4m) 1-83 200 AW 0.7, 0.001 Hz, 85,400s Note (1)

C264 (40 MPa4m) 1-83 175 AW 0.7, 0.001 Hz, 85,400s.-- 0 Note (2)

C26 .4 (40 MPaqm) 8, 1-84 1 -5-6 AW 0.7, 0.001 Hz, 85,400s .... 0 Note (3)

C265 (40 MPaA/m) 1-87 150 AW+TCP 0.7, 0.001 Hz 3.5 x 10-8

C265 (40 MPa4m) 1-87 150 AW+TCP 0.6, 0.003 Hz 11 --> 1.6 x 10-8

C265 (40 MPaqm) 1-88 150 AW+TCP 0.5, 0.003 Hz 3.3 x 10-8

C265 (40 MPagm) 1-88 150 AW+TCP 0.5, 0.001 Hz + 3000s 2 —› 0 x 10-9

C265 (40 MPa\lm) 1-89 150 AW+TCP 0.7, 0.001 Hz 20 —> 0.1 x 10-9

C266 (40 MPaqm) 1-94 150 AW+LRO 0.7, 0.001 Hz . 1 x 10-8

C266 (40 MPa\lm) 1-94 150 AW+LRO 0.6, 0.003 Hz 1 —> 0.1 x 10-7

C266 (40 MPaqm) 1-94 150 AW+LRO 0.5, 0.003 Hz 2.5 x 10-8

C266 (40 MPagm) 1-95 150 AW+LRO 0.5, 0.001 Hz ,--- 1 x 10-8

October 2, 2006 GE Final Report


C266 (40 MPa4m) 1-95 150 AW+LRO 0.5, 0.001 Hz + 3000s :--: 3 —) 0 x 10 -9

C266 (40 MPaqm) 1-96 150 AW+LRO 0.7, 0.001 Hz 1.6 -.> 0 x 10-8

C268 (22 MPaqm) 1-100 150 AW+TCP 0.5, 0.001 Hz .-- 3 x 10-9

C268 (22 MPa4m) 1-100 150 AW+TCP 0.4, 0.001 Hz 4 --> 2 x le -

C268 (22 MPaNlm) 1-100 150 ' AW+TCP 0.3, 0.01 Hz 2.7 x 10-9

C268 (22 MPaqm) 1-101 200 AW+TCP 0.3, 0.01 Hz Note (1)

C268 (22 MPaqm) 1-101 175 AW+TCP 0.3, 0.01 Hz .-,-, 0 Note (2)

C269 (22 MPa4m) 1-105 150 AW+LRO 0.5, 0.001 Hz 1.3 x 10-8

C269 (22 MPa4m) 1-105 150 AW+LRO 0.3, 0.01 Hz 4 x 10-9

C269 (22 MPa\im) 1-106 200 AW+LRO 0.3, 0.01 Hz Note (1)

C269 (22 MPaqm) 1-106 175 AW+LRO 0.3, 0.01 Hz ,--- 0 Note (2)

* Figures listed as 1, 2, 3... are from this report; Figures 1-71, 1-72, 1-73... are from Ref [1] ** R/v/hold = load ratio (K max/Kmin), frequency in Hz, and hold time at K max TCP = 650°C for 200 hours; LRO = 550°C for 10 hours

Note (1) - c263/c264/c268/c269 shows negative crack growth at 200 °C, probably related to Ni metal stability in the deaerated crack, which requires only small levels of H2 at 200 °C [2,3].

Note (2) - c263/c264/c268/c269 shows no crack growth at 175 °C, but there is concern for a residual effect of Ni metal stability producing crack shortening as described in Note (1).

Note (3) - c263/c264 shows no crack growth at 150 °C, but it had previously and no efforts were made to "reactivate" the crack after returning to 150 °C.

Table 2b — Representative Crack Growth Rates for Welded Alloy 22 *

Data from Table 2a that is considered most representative of the (near) constant K response

Specimen ID Figure* Temp., Heat Loading, CGR, (K) °C Treatment R/v/hold Minis

C263 (40 MPa\lm) 1-74 150 AW 0.7, 0.001 Hz, 85,400s 1.2 x 10-9

C264 (40 MPa4m) 1-82 150 AW 0.7, 0.001 Hz, 9000s 1.3 x 10-9

C265 (40 MPagm) 1-89 150 AW+TCP 0.5, 0.001 Hz + 3000s 2 x 10-9

C266 (40 MPa4m) 1-96 150 AW+LRO 0.5, 0.001 Hz + 3000s 3 x 10-9

C268 (22 MPaqm) 1-100 150 AW+TCP 0.5, 0.001 Hz 3 x 10-9

C269 (22 MPaqm) 1-105 150 AW+LRO 0.5, 0.001 Hz 1.3 x 10-8 *

* Note that all growth rates include cycling, and even then the cracks usually slow and arrest. c268 and c269 have fairly aggressive cycling, and their rates with >3000s hold time would be

much lower (esp. c269), so a representative growth rate for c269 is 3 x i0 mm/s.

October 2, 2006 GE Final Report


Table 3— Crack Growth Rates for Ti Grade 28/29 CT Specimens

Specimen c288 grew faster and was removed to permit further evaluation of specimen c287

c143, c144 = Ti Grade 7, Solution = BSW

c287 = Ti Grade 29, c288 = Grade 28, Solution = SCW

Crack growths in as-rec'd Ti Grade 7 (c143) are consistent with creep crack growth in air

Specimen ID (K) Heat Treatment Loading, R/v/hold** Temp, °C CGR, mm/s

C143 (30 MPaqm) As-rec'd 0.7, 0.001 Hz, 9,000s 110°C 4 x 10-8

C143 (30 MPaqm) As-rec'd 0.7, 0.001 Hz, 85,600s 110°C 1.3 x 10-8

C143 (30 MPaqm) As-rec'd Constant K 110°C 1.25 x 10-8

C148 (30 MPa4m) 20% CW 0.7, 0.001 Hz, 9,000s 110 °C 1.4 x 104

C148 (30 MPagm) 20% CW 0.7, 0.001 Hz, 9,000s 110°C 7.3 x 10-9

C148 (30 Milaqm) 20% CW 0.7, 0.001 Hz, 85,600s 110°C 7 x 10-' °

C148 (30 MPaqin) 20% CW 0.7, 0.001 Hz, 85,600s 110°C 2.5 . leo -

C148 (30 MPaqm) 20% CW 0.7, 0.001 Hz, 85,600s 110 °C* *1.4 x 10-1°

C287 (27.5 MPagm) As-rec'd 0.7,0.001 Hz, Os 150 °C 2.2 x 10'

C287 (27.5 MPagm) As-rec'd 0.7, 0.001 Hz, 9000s 150 °C 7.5 x 10-8

C287 (27.5 MPailm) As-rec'd 0.7, 0.001 Hz, 85,600s 150 °C 2 x 10-8

C287 (20 MPaqm) As-rec'd Constant K 150 °C 5 x 10-9

C287 (27.5 MPaNlin) As-rec'd 0.7, 0.001 Hz, Os 150 °C 2.5 x 10-7

C287 (27.5 MPa4m) As-rec'd 0.7, 0.001 Hz, Os 100 °C 8.5 x 10-8

C287 (27.5 MPaqin) As-rec'd Constant K 100 °C 3 x 10-9

C288 (27.5 MPagin) As-rec'd 0.7, 0.001 Hz, 9000s 150 °C 2.7 x 10-7

C288 (301' MPaqm) As-rec'd 0.7, 0.001 Hz, 85,600s 150 °C 3.7 x 10-7

C288 (331' MPa\lm) As-rec'd Constant K 150 °C 3.8 x 10-7

C288 (371' MPaqm) As-rec'd Constant K 150 °C 4.9 x 10-7

C288 (341 MPagin) As-rec'd Constant K 150 °C 1 x 10'

C288 (301 MPaqm) As-rec'd Constant K 150 °C 6.6 x 104

C288 (.--.35 MPagin) As-rec'd Constant K 150 °C 1.1 x 10-7

** R/v/hold = load ratio (Kmax/K), frequency in Hz, and hold time at K m. * With PbNO3 added to the environment



Table 4— Project Supplied Double U-Bend Specimens

Arm Spread Arm Spread Identification Heat Condition

Before Test After Test*

DUB1181(outer) / DUB1061(inner) 2277-9-3241 As-received 0.998" 0.975"







DUBI188(outer) / DUB1068(inner) 2277-9-3241 As-received 1.005" 0.973"


DUB I 190(outer) / DUB1070(inner) 2277-9-3241 As-received 1.006" 0.972"

* — dimension shown for inspection after 415 lhours; at that time, all U-bends were re-tightened as shown to compensate for possible stress relaxation.



Table 5— GE GR Single U-Bend Specimens

Identification Heat Condition* 1

C22 (227793263) TCP No. 1 2277-9-3263 TCP No. 1

C22 (227793263) LRO No. 1 2277-9-3263 LRO No. 1

Ti Grade 29 (956205) AR No. 1 *2 956205 AR No. 1

C22 (227793263) TCP No. 2 2277-9-3263 TCP No. 2

C22 (227793263) LRO No. 2 2277-9-3263 LRO No. 2

C22 (227793263) AR No. 2 2277-9-3263 AR No. 2

Ti Grade 29 (956205) AR No. 2 *2 956205 AR No. 2

C22 (227793263) LRO No. 3 2277-9-3263 LRO No. 3

C22 (227793263) AR No. 3 2277-9-3263 AR No. 3

C22 (227793263) TCP No. 4 2277-9-3263 TCP No. 4

C22 (227793263) LRO No. 4 2277-9-3263 LRO No. 4

C22 (227793263) AR No. 4 2277-9-3263 AR No. 4

C22 (227793263) TCP No. 5 2277-9-3263 TCP No. 5

C22 (227793263) LRO No. 5 2277-9-3263 LRO No. 5

C22 (227793263) AR No. 5 2277-9-3263 AR No. 5

C22 (227793263) TCP No. 6 2277-9-3263 TCP No. 6

C22 (227793263) LRO No. 6 2277-9-3263 LRO No. 6

C22 (227793263) AR No. 6 2277-9-3263 AR No. 6

Ti Grade 29 (956205) AR No. 3 956205 AR No. 3

Ti Grade 29 (956205) AR No. 4 956205 AR No. 4

*1 — machined U-bends after heat treatment below from customer supplied C-22 welded plate HT 2277-9-3263. The weld was located at middle of 6" dimension.

AR = as-received (as-welded) TCP (topologically close packed) = 650C for 200 hrs with water quench LRO (long range ordering) = 550C for 10 hrs with water quench

*2 — Two specimens removed to make space for the four new U-bends of Ti Grade 29: C22 (227793263) TCP No. 3 and C22 (227793263) AR No. 1.



Table 6— U-bend Inspection Results

17,241 hours of exposure on September 29, 2006

Ti Grade 29 U-bends started on May 19, 2006 and have 3185 hours of exposure on Sept 29, 2006

Date of Inspection Hours at Inspection Findings October 31, 2003 0 hours Start of test January 29, 2004 2166 hours No cracks observed *1

May 5, 2004 4151 hours No cracks observed *1 July 19, 2004 5588 hours No cracks observed *1

January 31, 2005 9,785 hours No cracks observed *1 March 29, 2006 14,056 hours No cracks observed *2 October 2, 2006 17,241 hours No cracks observed *2

*1 — AR-6 (as received) and TCP-1 (HT TCP) showed microscopic surface imperfections perhaps related to dissolution of inclusions, but no evidence of SCC.

*2_ Some double U-bends showed pitting on outer arm of outer specimen, but no crack. Some double U-bends taken apart, and crevice corrosion was observed in one case.



Table 7— U-bend Pit Dimensions

DUB1189-12ARM 10-12-05 DUB1182-50peak 10-12-05 maximum maximum

pit size diameter pit depth pit size diameter pit depth

(pm) (pm) (pm) (pm) (pm) (pm)

1 102 131 10 1 57 66 16

2 26 30 7 2 71 100 20

3 84 93 10 3 34 37 10

4 25 27 8 4 33 40 8

5 45 • 54 8 5 48 56 10

6 63 79 11 6 51 54 14

7 24 26 7 7 44 51 11

8 20 21 5 8 61 81 11

9 57 61 8 9 52 57 13

10 62 70 8 10 39 46 9

11 53 64 9 11 26 29 7

12 117 167 14 12 80 109 15

13 36 39 8 13 48 57 11

14 39 42 8 14 50 55 11

15 27 29 4 15 23 26 5

16 39 42 6 16 34 38 6

17 37 50 7 17 28 31 10

18 20 22 3 18 33 37 11

19 22 23 6 19 53 65 9

20 42 46 8 20 51 63 11

21 87 111 12 21 56 72 14

22 36 40 9 22 88 135 14

23 99 124 9 23 17 19 4

24 73 83 10 24 29 31 8

25 21 24 4 25 56 70 10

26 22 24 6 26 31 33 6

27 28 30 5 27 23 25 10

28 61 74 10 28 28 31 10

29 38 42 8 29 67 79 11

30 29 31 10 30 95 117 15

31 37 47 11 31 59 64 13

32 10 11 7 32 66 82 11

33 6 6 1 33 44 50 7

34 54 65 13



Table 8- Specimen Changes to Keno Test

Specimens removed from KENO to install 16 New Ti specimens (below)

Specimen Number Material Stress 75 316 65 ksi 134 316 65 ksi 111 316 65 ksi 18 316 65 ksi 44 316 65 ksi 157 C22 93 ksi 6 C22 93 ksi

16 New Ti specimens Added to KENO Test on June 8, 2006

105 °C Yield Strength Values Used: 40.7 ksi for Ti Gr.7 and 105 ksi for Ti Gr.29

Stress, Spec. # Material Dia 1* Dia 2 Dia 3* Ball # Manifold Module MPa

208 Ti Gr.7 0.224 0.220 0.224 210 4 1 10 209 Ti Gr.7 0.224 0.220 0.223 210 93 1 22 210 Ti Gr.7 0.225 0.221 0.225 210 23 1 30 211 Ti Gr.7 0.227 0.220 0.225 210 43 1 48 212 Ti Gr.7 0.240 0.237 0.241 180 3 3 15 213 Ti Gr.7 0.240 0.237 0.239 180 319 3 23 214 Ti Gr.7 0.240 0.237 0.240 180 249 3 35 215 Ti Gr.7 0.241 0.237 0.242 180 63 3 38 216 Ti Gr.29 0.127 0.123 0.130 684 287 2 36 217 Ti Gr.29 0.136 0.130 0.134 612 15 2 32 218 Ti Gr.29 0.137 0.129 0.138 621 184 2 28 219 Ti Gr.29 0.137 0.129 0.135 621 18 2 24 220 Ti Gr.29 0.150 0.140 0.146 472 7 2 22 221 Ti Gr.29 0.146 0.140 0.150 472 226 2 17 222 Ti Gr.29 0.150 0.140 0.150 472 40 2 5 223 Ti Gr.29 0.150 0.140 0.146 472 241 2 4

* Diameter 1 and 3 are just outside of the radius, and measurements are made to ensure that there is no undercut near the radius. The relevant specimen diameter is Diameter 2.



Table 9- CT String of Crack Initiation from Defected Specimen

Precrack

Target Crack Actual a/VV Specimen

Initial File Condition Stress a W Beff Beet Bgrosa ID# Length a/VV

Name

CTS1 #1 C22 As-welded (AW) higher K (30 kshlin) alW = 0.554 0.5549 0.4061 0.3720 0.9160 0.4759 0.4530 0.5000

CTS2 #2 C22 As-welded (KW) lower K (20 ksigin) aNV = 0.420 0.42004 0.4056 0.3725 0.9185 0.4749 0.4510 0.5000

CTS3 #3 C22 As-welded (AVV) lower K (20 ItsWin) aNV = 0.420 0.42005 0.4077 0.3745 0.9185 0.4745 0.4530 0.4970

CTS4 #4 C22 As-welded (AVV) higher K (30 ksiqin) alW = 0.554 0.55505 0.4150 0.3725 0.8975 0.4724 0.4500 0.4960

CTS5 #5 C22 AW+TCP higher K (30 kshlin) alW = 0.554 0.55499 , 0.4163 0.3730 0.8960 0.4754 0.4530 0.4990

CTS6 #6 C22 AW+TCP lower K (20 ksigin) aNV = 0.420 0.42021 0.4085 0.3730 0.9130 0.4749 0.4620 0.4990

CTS7 #7 C22 AW+TCP higher K (30 ksnlin) aNV = 0.554 0.55525 . 0.4087 0.3760 0.9200 0.4759 0.4530 0.5000

CTS8 #8 C22 AW+TCP lower K (20 ksiqin) a/W = 0420 0.42018 0.4036 0.3715 0.9205 0.4755 0.4540 0.4980

C22 AW+SHT +Water CTS9 #9 higher K (30 ksigin) a/W = 0.554 0.55494 0.4074 0.3720 0.9130 0.4729 0.4490 0.4980 Quenched

C22 AW+SHT +Water CTS10 #10 lower K (20 ksi ,lin) aNV = 0420 0.42909 0.4026 0.3700 0.9190 0.4765 0.4550 0.4990 Quenched

C22 AW+SHT +Water CTS11 #11 higher K (30 ksi4in) aNV = 0.554 0.55514 0.4059 0.3730 0.9190 0.4785 0.4580 0.5000 Quenched

C22 AW+SHT +Water CTS12 #12 lower K (20 ksigin) alW = 0420 0.42005 0.4045 0.3715 0.9185 0.4765 0.4550 0.4990 Quenched

CTS13 #13 C22 AW +SHT +Air blasted lower K (20 IcsiNlin) aNV = 0.420 0.42008 0.4107 0.3700 0.9010 0.4775 0.4560 0.5000

CTS14 #14 C22 AW +SHT +Air blasted higher K (30 kshlin) aNV = 0.554 0.55439 0.4133 0.3720 0.9000 0.4749 0.4510 0.5000

C22 AW +SHT +Still air CTS15 #15 higher K (30 ksi,/in) a/W = 0.554 0.55426 0.4121 0.3715 0.9015 0.4743 0.4500 0.5000 cool

C22 AW +SHT + Still air CTS16 #16 lower K (20 Icsblin) aAN = 0.420 0.42011 0.4054 0.3730 0.9200 0.4739 0.4630 0.4990 cool

CTS17 #17 C22 Base lower K (20 ksi.lin) a/W = 0.420 0.42018 0.4056 0.3725 0.9185 0.4744 0.4510 0.4990

CTS18 #18 C22 Base higher K (30 ksiqin) a/W = 0.554 0.55431 0.4065 _ 0.3740 0.9200 0.4749 0.4510 _ 0.5000

Total load on 0.5TCT specimen is 1235 pounds to achieve indicated K

SHT = 1120C /30 minutes / water quench unless otherwise specified As-welded = pnscrack in weld metal

AW + TCP = precrack in weld metal, heat treat at 700 C / 175 hours AW + SHT with water quench, precrack in weld metal

AW + SHT with still air cool down, precrack in weld metal

AW + SHT with air blast cool down, precrack in weld metal

As-received material, fatigue crack not in weld metal

If not all conditions can be accommodated, the air blast cool down condition.

Testing: - Test started on June 5, 2006 at 2:00 pm 6/5/2006 7/14/2006 39.00 936 hours



Table 10. Nominal Chemical Composition of Ti Alloys

Chemical Composition (wt %

Fe Ni Cr Ru Al C V , Pd Ti

Ti Grade 23+Pd 0.17 0 0 0 6 0.01 4 0.07 89.75

Ti Grade 29 0.18 0 0 0.112 6.05 0.02 0 . 0 93.64

Ti Grade 7 0.3 0 0 0 0 0.006 0 0.2 98

AKOT 0.05 0.44 0.16 0.032 0 0.008 0 0.01 99.25

Table 11. Chemical Composition of the Test Solutions (Molal)

ID Temp. pH CaCl2 KCI KNO3 NaNO3 NaCI Na2SO4 NaF NaBr

TS-1 150 4.9 3.6 5.8 1.8 2 0 0 0 0

TS-2 120 7.3 0 7 0 1.8 1.2 2.4 0 0

TS-3 120 9.0 0 7.2 0.3 3.3 0 2.1 0.2 0

TS-4 150 9.7 0 5 2.8 6.6 0 6.8 0.1 0.1

TS-5 120 4.9 3.6 5.8 1.8 2 0 0 0 0

Table 12. Hydrogen Pick-up by Ti Alloys

H2 Takeup by Fresh Surface (wt%)

Before TS1 TS2 TS3 TS4

Test Alloys Immersion

Ti Grade 23+Pd 0.0142 0.0138 0.0148 0.0151 0.0143

Ti Grade 29 0.0049 0.0042 0.0054 0.0044 0.0048

Ti Grade 7 0.0018 0.0013 0.0016 0.0018 0.0016

AKOT 0.0036 0.0038 0.0037 0.0038 0.0037

H2 Takeup by Oxidized Surface (wt%)

Before TS1 TS2 TS3 TS4

Test Alloys Immersion

Ti Grade 23+Pd 0.0142 0.0138 0.0147 0.0142 0.0131

Ti Grade 29 0.0049 0.0045 0.0046 0.0049 0.0048

Ti Grade 7 0.0018 0.0024 0.0016 0.0019 0.0019

AKOT 0.0036 0.0038 0.0040 0.0038 0.0025



Table 13. Corrosion Rate of Ti alloys

Corrosion Rate, um/year

Fresh Surface in TS-1 Oxidized Surface in TS-1

EIS CPP Weight Loss EIS CPP Weight Loss

Ti Grade 23+Pd 3.539 0.760 0.409 3.388 0.667 0.585

Ti Grade 29 2.339 0.238 0.528 2.029 0.632 0.499

Ti Grade 7 2.533 0.301 0.286 1.956 0.186 0.176

AKOT 1.989 0.329 0.192 1.433 0.208 _ 0.255




Ti Grade 23+Pd 1.298 0.111 0.351 1.936 0.102 0.351

Ti Grade 29 1.010 0.082 0.235 1.659 0.090 0.235

Ti Grade 7 1.772 0.248 0.501 0.726 0.309 0.316

AKOT 2.020 0.216 0.319 0.914 0.268 0.447




Ti Grade 23+Pd 2.150 0.120 0.292 1.889 0.130 0.351

Ti Grade 29 1.044 0.084 0.264 1.337 0.101 0.235

Ti Grade 7 1.581 0.256 0.608 1.581 0.309 0.563

AKOT 2.194 0.208 0.511 1.512 0.329 _ 0.319



EIS CPP Weight Loss EIS CPP Weight Loss _ . Ti Grade 23+Pd 1.703 0.213 0.643 5.137 . 0.250 0.526

Ti Grade 29 1.426 _ 0.165 0.382 _ 2.988 0.229 0.293

Ti Grade 7 2.884 0.080 , 0.251 0.693 0.115 0.246

AKOT 1.065 0.104 0.192 1.310 0.069 0.383


1

11.7

1.6

EE 11.51

11A

co 113

11.2

2.2x 10

mmts

to

4. -o.1 11.8 1 CT potential 2 x 10-8 malls

2000

-1- -i

2560

o

-0.1

- -0.2 . 0

. 0 - -03 7x 10"ar1rnis

2000

11.75 -1--

1800 22:0 2903 30:0

-I-_I

3230


11.9 -t

SCC#1 - c287 - Ti Grade 29, heat 956205

=0.7

, 0

.00

1 H

z @

49

h

11.1

11

10.9

N

0) 0 °. 0 .0 rz.

8 0

E. 0

8 x 10-8

innYs

7.5 x 10

rnnts - -02

0 •to o

4S'

--03 t

,_, co • us 0

@ • c : E

F---C . 0

- -0.5

'El • rt

a 8 o 0

--06 a4,i E-ott.

tO . To co

• « • o

7 .0.8

-0.9

c287- 0.5TCT of Ti Grade 29

25 Icsbiin, SCW Water, 150C

500 1000 1500

Test Tune, hours

Figure 1. Crack length vs. time for Ti Grade 29.

SCC#E - c287 - Ti Grade 29, heat 956205

11.83

11.82 CT potential

11.81

E- .8 6-1 go3

mrs 4044.41114- :

c

co E -

/

11.79 2 x 1 0

m

: c 71. -8 cq • E

tci 7 -0.6 cg 6-

11.78 E.7. ii. ... T. 6- + a . 0 11.77

8 . a.

0 c287 - 0.5TCT of Ti Grade 291 - -0.8 E.

11.76-f _ NI 25 Icshlin, SCWINater, 150C

2400 2030

Test Tiny, hours


-as


0 0 CD CD

CD

16.2

ksh

lin

@ 5

.00

h

1.0 x 10'e mm/s

5100 5600

22 k

sh

iln

411

3600

h

17

.6 k

siq

in @

45

0

19

.7 k

shil

n @

40

00

h

1.9 x 10-9 mrrils

l3.2 -J

124. 1.8x10 °

mm/s

11.81 I



11.861 . I

Po

ten

tial

vs.

Pt

refe

ren

ce e

lectr

od

e ..g

11.85 -I-

11.84

c 11.83

2 1 1

11.82 +

11.81 +

11.8 -I-.

2600

CT potential

cri

CD

uCD

- go)

o

5 4..

01 CO 0 0 I. I

Zi; 0 QC CD

g

4.6 x lemm/s

6 x 10-9 mrrils

3100 3600 4100 4600

co

-0.2

-0.3

1. -0.4

-0.5

-0.6

-0.7

-0.8

-0.9

6100

To

Con

sta

nt

K @

23

95

h

c287 - 0.5TCT of Ti Grade 29

25 ksiqin, SCW Water, 150C

Test Time, hours



Coole

d t

o 1

00

C (

kt 76

60

h

CT potential

134

2.5 x 104

mmls

- W

xo 6

01 t 8

0

u 12.4 Jo a o r: 0 ,. u I ,.

12.2-t 1



5900 6100 6300 6500 6700 6900 7100 7300 7500

Test Time, hours


ei fl, E12.8 E

0 .5, 0 to 6 o) _ _ .9. C'l tol o)

1

-0.2

-0.3 0

To -.0.4 S

-0.5

a.

--0.6 ch

:

-0.7 .45 0.

-0.9

-1

7700


13.7

2.7 x 10-8

mmls

6.5 x 104

mm/s

Jak CT potential Gs

t•••

"a

0

8


25 ksi -qin, SCW Water, 150C

3x 10-9 mrnis

13.65

13.6

13.55

E

•

13.5

c 13.45

12000 13000

o co 13.4

13.35- '

13.3- 8 : 0

r••

13.25- It.: . 0 o • n o

13.2 • •

7000

10

0C

0 7

660

h

9000

3 4° GO O ts

• (4. 8

S o

11000 10000

7 -0.1

-0.2

7

•

-0.3

0

- is

- -0.5

: E

-.0.6 r: 15 •

--07

o.

7 -0.8

-0.9

~~-1

SCC#1 - c288 -11 Grade 28, heat 870749601

• -0.1

-02 ,

• - -0.3 t : • 'Li

--0.4 3 • c

-0.5 in re

1. -° 6 -0.7 c

o:76° 1-0.8

E

•

12.44

cn

co 11.9

27 k

sh

/in

CO

1800

c49 @

"0 0.0

CI4 8 0O E. ‘t

I0 co

29 k

sbli

n 0

2300

h


25 icshlin, SCW water, 150C

500 1000

1 -0.9

i • -1

2000 2500 0 1500



Test Time, hours


Test lime, hours



4200 4400

15 t

14.9


6.6 x 10-8 mmt CT potential 1-0. 1

27 k

sW

in @

4394

h

28 l

ish

lin

@ 4

196

h 7 -0.2

,

- -0.3 43 :

ru- - -0.4 3 •

--0 . 5 15 • re

f -0.6

1- -0.7 E '70

11: -0.8

1 -0.9

-1

Observed data under

-dl<kla conditions

2.2E-07

2.0E-07

1.8E-07 L.

E

•

1.6E-07 -- E

4.11 co 1.4E-07 -

CC

e 1.2E-07 7

t) 1.0E-07

8.0E-08

6.0E-08


25 kstgin, SCW Water, 150C

•••••".. •••••• I •

•••••

1-•70-••-•--1

/ .

/ .:‘

/ K6

/

/ • /

7 4... 4

/ K• ... / • '.

...- - .-- -

/ • /

., .- ...... K3

• ....• . ...* ..--

/- - ..-- '''' 7

• • ....- . ...- .


ati 03 tl) C0 C* gl

14.8 - 2

• co -2

. to es 44 • 14.7 " cei

-

31 k

sh

lin

@ 3

686

h

8x 10'e mmis

30 k

abil

a @

3825

h

29 k

shii

n @

4010

h

1 x 10-7 MITI'S

ti c I 2J -4 co

(..) z i) ial

5. = ' 14.5+ / t rj C.1

S 12. '', te

14.4 -I- / 4.9 x 10-7 2.71

RIM'S

lb

14.3 " "



3200 3400 3600 3800 4000

Test Time, hours



4.0E-08

30 31 32 33 34 35 36 37 38 39 40

Stress Intensity Factor, MPaqrn

Figure 8. Crack growth rate vs. stress intensity factor for Ti Grade 28.


Cra

ck G

row

th R

ate

, m

m/s

9.E-09

8.E-09

7.E-09

6.E-09

5.E-09

4.E-09

3.E-09

2.E-09

1.E-09

0.E+00

12

1.E-08

14 16 18 20 22 24 26 28 30

Stress Intensity Factor, MPa4m

Figure 9. Crack growth rate vs. stress intensity factor for Ti Grade 29.



"

••••••

•

' " ' I ' " I " '

Observed data under

-d1</da conditions r•-••

/ .

/ ? . _ K6 /

/ .

/ K4 '

/ / 7

C.

3 / f K ,

/

/ / .0

co

12

2 0

cci

1.E-06

1.E-07

1.E-08

SCC of 20% Cool Worked Stainless Steel

288 °C, 2000 ppb 02, Pure Water

0 5 25 30 20



10 15

Stress Intensity, kshlin

Figure 10. Crack growth rate vs. stress intensity factor for 20% cold worked type 316L SS.


1.E-06

//)

2

1.E-08

10 12 14 16 18 20

Stress Intensity Factor, ksi4in

8 26 24 22

1.E-06

_ 1.607

1.E-08 f • • • f f • • • I

28 26 30


1.E-07

Effect of Stress Intensity Factor (K) on

Crack Growth Rate of 20% Cold Worked

316L SS Tested in 288 C Water Using

A Very Slow Reduction in K Under

"Constant K" Conditions (No Cycling)

Figure 11. Crack growth rate vs. stress intensity factor for 20% cold worked type 316L SS.

Effect of Stress Intensity Factor (K) on

Crack Growth Rate of 20% Cold Worked

• Wrought Alloy 182 Tested in 288 C Water

• Using A Very Slow Reduction in K Under

"Constant K" Conditions (No Cyding)

I. K15 Dependency

14 16 18 20 22 24

Stress Intensity Factor, MP-64m

Figure 12. Crack growth rate vs. stress intensity factor for cold worked type 316L SS.


7000 9000 11000 13000 15000 17000 19000 21000 23000

R=0.7, 0.001Hz + 85,400s hold @ 6446h 8 v CI 0

4+ CV 0 I° CI GI

IC tal

0 —0 mrn/s cu 0

I> 0 hi

SCC of c263 - Alloy 22, As-welded, 150C

40 MPaqm, Air sat'd, SCW Chemistry

24.39 -{ SCC of c264 - Alloy 22, As-welded, 150C


R=0.7, 0.001Hz + 85,400s hold @ 6446h

-0 mm/s

210

.0 0)

8

0

0

t:14)

El ...I V

° ny a 41_1

24.32

24.31

24.3

7000 9000 11000 13000 15000 17000 19000

Time, hours

24.38

24.37

E 24.36

to. c 24.35

0;$ 24.34 — fl)

24.33 ;7' @ g 8

UO E.

180

1 0.

170

1 160

t 150

• • 1 140

21000 23000

I 200

190


SCC#4 m of c263 - Alloy 22, as-welded

Time, hours

Figure 13. Crack length vs. time for Alloy 22, As-welded.

SCC#4m of c264 - Alloy 22, as-welded 4 . . I . . . 24.4 220

Figure 14. Crack length vs. time for Alloy 22, As-welded.


24.78 .

- 24.77 -

• 00

• A co

24.76-

E

E 24.75- 4:;.

c 24.74 -

.x •

s- 24.73 - C.)

SCC#4m of c265 - Alloy 22, as -welded +TCP

-1 x10 10 mmis +152

150 E a

1443 ,12

- 146

144

142

' 140

13500 14500 15500

24.71

24.7 " ' " " ' " •

8500 9500 10500 11500 12500

SCC of c265 - Alloy 22, AW+TCP, 150C

40 MPalim, Air sat'd, SCW Chemistry

7 160

158

156

154

12000 14000

Time, hours

1,....■■■■•■■■

10000 16000


Time, hours

Figure 15. Crack length vs. time for Alloy 22, As-welded + TCP.

SCC#5m of c265 - Alloy 22, as-welded +TCP

0 0 a .4

C4 CD

d

SCC of c265 - Alloy 22, AW+TCP, 150C


.17

g

*g

g tit a. E

"

18000 20000

5 x 104

minis / -156

"- 154

.8 - - 152 0

a

so E

• -148 g

o•

§ 146

o "

• 144

142

140 111■1■11.

22000

Figure 16. Crack length vs. time for Alloy 22, As-welded + TCP. Note that Figures 1-89 and 1-90 in the 2005 Final Report [1] was incorrect in showing a change to constant K at 9772 hours.


25.2 7-

25.15

25.1

25.05

E 25 -

0 C 24.95 -

12 24.9 7

24.85

24.8 -

24.75

24.7

8000

158

156

f 154

-I. 152

150 12 0 o.

148 12

146

SCC of c266 - Alloy 22, AW+LRO, 150C

40 MPaqm, Air saVd, SCW Chemistry

24.55 +

24.5

144

142

- 140

111

0 CO

6 et 24.75

II

24.7 E.

-0 mm/s

24.8 160

-0 mm/s

c 24.65 ca

ti)

to

24.6

24.9 t

24.85 I

24.8

24.75

E

•

24.7

c 24.65 - as

Je

03 24.6 -

a 24.55

24.5 -[

2445-f

24.4 -f—s—.—s—r

8000 10000 12000 14000 16000 18000

Time, hours

r4

0 0 0 ci

t*:

-0 mm/s

.0 mm/s

El 11

E 1,1

tu t

I . 160

158

156

150 E o.

148 15!

oi

146

-8 • .o 144

• 0

§ 142

E. t • 140

20000 22000

SCC of c266 - Alloy 22, AW+LRO, 150C

40 MPagm, Air sat'd, SCW Chemistry

154

152 C-)


SCC#4m of c266 - Alloy 22, as-welded +LRO

9500 10500 11500 12500 13500 14500 15500

Time, hours

Figure 17. Crack length vs. time for Alloy 22, As-welded + LRO. Note that Figures 1-96 and 1-97 in the 2005 Final Report [1] was incorrect in showing a change to constant K at 9772 hours.

SCC#5m of c266 - Alloy 22, as-welded +LRO

8500

Figure 18. Crack length vs. time for Alloy 22, As-welded + LRO.



Figure 19. DUB-1182 Exterior Surface of Outer U-bend Arm

Figure 20. DUB-1066 Creviced Region Outside of U-Bend


Keno Testing (Full Run 2) Occ06

Concentrated Salt Solution 105 °C

Constant Stress; 201 specimens total

2.5 +

316NG

;a 2.0 1-

>-

1 -6. a

Creviced and uncreviced ii Gr.7 and sensitized SS

Ti Or 7

Pressure increased from 8.67 MPa

to 10.3 MPa at 168.5 hrs

• oys .,,„ used in stress ratio for welded specimens

5000 10000 15000 20000 25000

Time-to-failure (hrs)

1.0

113

Notched Alloy 22 11:

Alloy 22

0.5

0

Ti Gr 7 as received

• Ti Or 7 creviced

• Ti Gr 7 as received

• Ti Or 29 as received

Ti Gr 7 failure at I 1156YS

at >5000 hours


• Alloy 22 as received

• Alloy 22 creviced

0 Alloy 22 HT1 (TCP)

X Alloy 22 HT1 +creviced

• Alloy 22 HT2 (LRO)

• Alloy 22 20% CW

• Alloy 22 20%CW +LRO

Alloy 22 weld + HAZ

• 316NG as received

• 316NG creviced

0 Ti Gr 7 as received

• Ti Or 7 creviced

X 304 SS sensitized

• 304SS sens + creviced

• Notched A22 as-rec

• Notched A22 HT1 (TCP)

• Notched A22 weld+HAZ

Figure 21. Time to failure vs. %YS in 15% BSW solution at 105 °C.

2.0

Keno Testing (Full Run 2) cki.(6

Concentrated Salt Solution 105°C

Constant Stress; 201 specimens total 1.5-f

0

43a

1.0 —

I E

n

-2. 0;

0.5 — 8 specimens each of Ti Grade 7 and 29, each alloy tested at two stresses

(one Ti Grade 29 specimen is at a third, higher stress).

For yield strength, used 40.7 ksi for Ti Gr.7 and 105 ksi for Ti Gr.29.

Groups of four points are separated in %YS & Hours to improve visibility.

17- No failures have occurred in these 16 pink & blue specimens.

0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000

Time-to-failure (hours)

Figure 22. Time to failure vs. %YS for Ti specimens in 15% BSW solution at 105 °C.

•


700

600 7° 2

E a g

I. 1 500 %I *,

I.

I. 3

g 3 al 400 p

a. eh

2 D

co 300 13

200

(r) O 0. 0.

03 O. 7

0.1 ' 18

: Creep Test on Ti Grade 7, CNO171 184 -

"Short" Orientation

182

• ca

• 178

174

176

• • •

172 •

07

100 .

: Creep Test on Ti Grade 7, CNO171 . 184 -

"Short" Orientation .

. .

• ' ca .

' .

178 .

' .

' .

174

•

172

07

•.: .

'

'

"

0.

0.

0.

0.

0.t68lV

0

0

8 g

14

6

4

16

12

10

2

0.03 0.04 0.07 0.06


• —>

Ti Gr 7 as received

A Ti Gr 7 creviced



Keno Testing (Full Run 2) Oct '06

Concentrated Salt Solution 105 °C Constant Stress; 201 specimens total

I --->

S

—>

Ti Gr 7 failure at 40 kW at >5000 hours

8 specimens each of Ti Grade 7 and 29, each alloy tested at two stresses

(one Ti Grade 29 specimen is at a third, higher stress).

For yield strength, used 40.7 ksi for Ti Gr.7 and 105 ksl for Ti Gr.29.

Groups of four points are separated In Stress and/or Hours to improve visibility.

No failures have occurred In these 16 pink & blue specimens.

0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000

Time-to-failure (hours)

Figure 23. Time to failure vs. applied stress for Ti specimens in 15% BSW solution at 105 °C.

Ti Grade 7 As-Rec'd 105C, Air, Creep Test #5

loo

0.02 0.05

Time, hours

Figure 24. Creep tests #5 on Ti Grade 7 in 105 °C air.

0.08


Creep Test on Ti Grade 7, CNO171

"Short" Orientation

Initial Loading at 0.005"/min

45

40

35

30

I.-. 20

*rn -lc 25

(/) C)

0.8

Strain, %

0.2 0.4 0.6 1.2 1.4 1.6

15

10

5

0

36

.7)

.1L

co

32

30

28

g34

ao

38


"Short" Orientation

Re-load from 800#

4 26

0.1 0.2 0.4 0.5


Ti Grade 7 As-Rec'd - 105C, Air, Creep Test #5


Ti Grade 7 As-Rec'd - 105C, Air, Creep Test #5 42

1.8

0.3

Strain, %


0.6


+1- 1 mm strain gage

attached just outside

of the autoclave

Actuator motion and strain gage give same

displacement at constant load creep conditions

0.5

Time in Hours

0 .c 0.2

.5 0.15

a. 0 0.1 5

0.05

0

0 0.25 0.75


111% of Yield Strength (42.5 ksi)

= 47.25 ksi ("short" orientation)

0.3i

0.25

T 300

+ 250

200

fn

150 .d

to.

+ 100

+50

0

40

39

38

37

36

35

:71 34

. 33

32

C7) 31

30

29

28

27

26

25

1.4 1.5 1.6 1.7 1.8 1.9 2

Strain, %

2.1 2.4 2.2 2.3 2.5 2.6





.. .....-

_7

/

..


114.7% of Yield Strength (36.0 ksi)

• = 41.3 ksi ("Long" Orientation) —

Initial Loading at 0.005"/min —



0.625" long gage section, so

0.1' displacement o 113% strain

Failure at

143.013 hr

025 t

a o.,

0. t

• ler.....„4Detioration with Arl

1p

100

Test Solution 1 at 150C

3.8m CaCt2 • Slim KCI • 1.8m KNO3 + 2m NaNO3

• 11 Grade 23+Pd: Fresh Surface

11 Grade 29: Fresh Surface

x Ti Grade 7: Fresh Surface

+ AKOT: Fresh Surface

10

• 11 Grade 23+Pd: Oxidized Surface

x T1 Grade 29: Oxidized Surface

• Ti Grade 7: Oxidized Surface

- AKOT: Oxidized Surface

35

0 57

a.

-100

30 15 20 25

400

-200

-300

0

300

— 200

005


0.3

Ti Grade 7 As-Reed - 105C, Air, Creep Test #6

O2 I

.c

E 0 151


114.7% of Yield Strength (36.0 ksi)

= 41.3 ksi ("Long" Orientation)

0 20 40 80 SO 100 120

Time, hours

Figure 29. Creep tests #6 on Ti Grade 7 in 105°C air.

Immersion Time, day

140

40

Figure 30. OCP of Ti alloys in TS-1 at 150 °C.


OC

P, m

V(0

.1N

KC

!, A

g/A

gC

I)

elirs 411,16

reiktrogNetere,1 am. gimilbtiP,

"Am op* tbie a•ao

100

[Doiteration with Ar

-100

1114: .711111,‘

#401167i opmiti

1151 f

oni

Viz iegftt

1

OC

P, m

V(0

.1N

KC

I. A

O/A

0C

I)

Doacratton with At

jAaration 1

10 15 20 25

Immersion Time, day

30 35 40 0 6

0 5 30 35


• n Grade 23+Pd: Fresh Surface

Ti Grade 29: Fresh Surface

Ti Grade 7 Fresh Surface

AKOT: Fresh Surface

• Ti Grade 23+Pd: Oxidized Surface

X Ti Grade 29: Oxidized Surface


AKOT: Oxidized Surface


7m KCI • 1.8m eloNO3 • 1.2m NO* 2.4m 1432504

10 15 20 25

Immersion Time. day


• TI Grade 23+Pd: Fresh Surface

• Ti Grade 29: Fresh Surface

x 71 Grade 7: Fresh Surface

+ AK07: Fresh Surface


x Ti Grade 29: Oxidized Surface

• Ti Grade 7: Chddlzed Surface

• AKOT: Oxidized Surface

.ts .05Cer*44**

ke, g1111%.,,,, ,,,, ,,„:.wispowl 414 ab4a liNfusvai*"1-Wa

-100

Tait Solution 3 al l20C

7.2m KCI • 0.3m KNO3 • 3.3m NaNO3 • 3 Na2SO4 • 0 N.3F

-200



40

.100

1.0E+06

1.0E+05

I 1.0E+04

• 1.0E+03

2

cc 1.0E+02

1.0E+01

li t

• Ti Grade 23+Pd: Fresh Surface


71 Grade 7: Fresh Surface

AKOT: Fresh Surface


x Ti Grade 29: Oxidized Surface



1.0E+00

1.0E-02

• • • • • • • • • .• • •

1.0E+01 1.0E+02

Frequency, Hz

• • • • • • • • • • • • • • • • •

1.0E+04 1.0E+05 1.0E-01 1.0E+00 1.0E+03

Report Number: GE—GRC—Bechte1-2006-2


v Ti Grade 29: Oxidized Surface




23m KNO3 • 6.6m KNO3 +6.8m Na2SO4 + 0.1m NaF + 0.1m NaBr

• T1 Grade 23+Pd: Fresh Surface


x T1 Grade 7: Fresh Surface


O 5 10 15 20 25

Immersion 'rime, day

with Ar I Sig .

4

AI 4iito q■ ..

30 35 40


4 4 000

......

6 ., m ilp

tif4 m lifi i e.,

li!gx •:igx

• •44

I 44xx x 44 44

44 4 4

" Wilitt illii i ..... I1 1111


3.6m CaCl2 + 5.8m KCI + 1.8m KNO3 + 2m NaNO3

Figure 34. Bode plots of impedance response of Ti alloys in TS-1 at 150 °C.


• TI Grade 23+Pd (FS)

• TI Grade 29 (FS)

Ti Grade 7 (FS)

+ AKOT (FS)

• Ti Grade 23+Pd (OS)

x TI Grade 29 (OS)

• Ti Grade 7 (OS)

- AKOT (OS)


7m KCI + 1.8m NaNO3 + 1.2m NaCI + 2.4m Na2SO4

aliffs 4.6ds

wil 844; d4 4. ligx_ *ids

1.0E+01 1.0E+02

Frequency, Hz

1.0E-01 1.0E+00

1.0E+00

1.0E-02 1.0E+05 1.0E+04 1.0E+03

1.0E+05

1.0E+04

• TI Grade 23+Pd (FS)

• TI Grade 29 (FS)

Ti Grade 7 (FS)

+ AKOT (FS)


x Ti Grade 29 (OS)

• TI Grade 7 (OS)

- AKOT (OS)

If 1.0E+03

.5

1.0E+02

1.0E+03 1.0E+00 1.0E-01

A • 1.1•1,

1.0E+01 1.0E+02

Frequency, Hz

1.0E+04 1.0E+05

1.0E+00 1--

1.0E-02


1.0E+06

P I !! . 1.0E+05

gil lit -t44 .MIS le e

1.0E+04

1 1/14

1.0E+02

1.0E+01

0 g 1.0E+03


1.0E+06

1.0E+01

• • ,•,,, Test Solution 3 at 120C

ill • e • • _ 7.2m KCI + 0.3m KNO3 + 3.3m NaNO3 + 2.1m Na2SO4 + 0.2m NaF

et* lit, 'Im o.

2IIZ g ee

Ml ifiliv ii i eepw-

if

itlig m

4

"Ili& w 4 I -6 d ilie 46 d

illi

if

4

Figure 36. Bode plots of impedance response of Ti alloys in TS-3at 120 °C.


0.0E+00

0.0E+00 4.0E+04 6.05+04

Z. real (ohm.cm2)

Fresh surface Test Solution 1 at 160C

3.6m CaCl2 +8.3m KCI + 1.8m KNO3 + 2rn NaNO3

' 6.0E+04

TI Grade 29

A • : :

TI Oracle 7

. •

Figure 38. Nyquist plots of impedance response of Ti alloys in TS-1 at 150 °C.


1.0E+06

• Ti Grade 23+Pd: Fresh Surface • Ti Grade 23+Pd: Oxidized Surface

..•••„ • Ti Grade 29: Fresh Surface x Ti Grade 29: Oxidized Surface

1.0E+05 4,:::ii .. • S • *Ti Grade 7: Fresh Surface • Ti Grade 7: Oxidized Surface

*x 4 o •

o _x x 44-r-f. xx •••• + AKOT: Fresh Surface - AKOT: Oxidized Surface -• om xxt#41,++8_,.. .41,

1.0E+04 r n om x + f.o ;-_ ! .. ro

- u m. 144 + 4. z * - - to

•11 X#4 4. +To '44 E " n om x4 11 +T x -s. .c

• 0 • *A -1..f.• •• 6 1.0E+03 .* . ....**$.4-:x., y •- . i - . ..'S*;++44x .- -.., . . ••••* 1g , re liwir:M x T x oe

e 1.0E+02 , •me:04 x ..

o

.1* II S. _

ipz... - Ii_tio

w °•'-.

1.0E+01 E ii..11h, •, - ..

."11114:11glfs. •• - - illifildiala$1004 11 9

- Test Solution 4 at 150C oll " 5m KCI + 2.8m KNO3 +6.6m NaNO3+ 6.8m Na2SO4+ 0.1m NaF + 0.1m NaBr

IIIIV

1.0E+00 - .

1.0E-02 1.0E+03 1.0E-01 1.0E+00 1.0E+01 1.0E+02

Frequency, Hz

1.0E+04 1.0E+05



• •

E 1.2E+05

NI° 5 8.0E+04

• 11 Grade 29

• •

•

11 Grade 7

6.0E+04

Z, real (ohm.cm2)

4.0E+04

0.0E+00

0.0E+00

• •

•

• • •

•• 1 Adat, I

2.0E+04 4.0E+04

AKOT •

• •

• •

• A • •

1.2E+05 1.0E+05 8.0E+04

•

4.0E+04

0.0E+00

0.0E+00

•

• •

• •

• • AKOT

2 • • • 11:0;07afti• • Ti Grade 7

3.0E+04

•

1.2E+05 9.0E+04


Fresh surface


7m KCI + 1.8m NaNO3 + 1.2m NaCI + 2.4m Na2SO4

2.0E+05

1.6E+05

• TI Grade 23+Pd


Fresh surface


7.2m KCI + 0.3m KNO3 + 3.3m NaNO3 + 2.1m Na2SO4 + 0.2m NaF

2.0E+05

1.6E+05

TI Grade 29

1.2E+05

itt 8.0E+04

•

TI Grade 23+Pd

•

•

6.0E+04

Z, real (ohm.cm2)



2.1E+06

1.8E+06

1.6E+06

Fresh surface


5rn KOl + 2.em KNO3 + 6.6m N3NO3 + 6.8m Na2SO4 + 0.151 NaF + 0.1m NaBr

* .1.2E+06

,fl Grade23+P .d

g 9.0E+04

8.0E+94.

: :•3 •0S+.04:•

3.0E+04 8.0E+04 8.0E+04 1.2E466 1.5E+06 131E+06 2.1E408 2.4E+05

Ph

ase A

ng

le, d

eg

ree

60

40

20

0

-20

-40

-60

.80

-100



• • . -

•

A • i•

••:h •• x•

• •

l• • • •1,

• Ti Grade 23+Pd: Fresh Surface





x11 Grade 29: Oxidized Surface

• 11 Grade 7: Oxidized Surface


Test Solution 1 at 150C 3.6m CaCi2 + 5.8m KCI + 1.8m KNO3 + 2m NaNO3

I ■ ••N • ••ii ••N

..

••ix ••i x • -

• 41

••4 x .

••iii x • • AIN x • -

41 x •• - Ai- z

A , -

zxxx- •el • - M ,

e x

..

11XXI?(`X- 11, X t

• lit ii. * X XX XX x

iiii ass milimm 4

1/ v • 141. x x •••

x • le xxxx x •

. 4 4 mmmm mmm AgiiiiiiiiiiiiiIIIIIMM 4664 6** . 466 ********** 66666 11,664444$110;i4-

• I ••I•1 • • •I• LI

1.0E-02 1.0E-01 1.0E+00 1.0E+01 1.0E+02 1.0E+03 1.0E+04 1.0E+05

Frequency, Hz

Figure 42. Phase angle plots of impedance response of Ti alloys in TS-1 at 150 °C.


• Ti Grade 23+Pd (FS)

• Ti Grade 29 (FS)

Ti Grade 7 (FS)

+ AKOT (FS)

• 11 Grade 23+Pd (OS)

x Ti Grade 29 (OS)

• 11 Grade 7 (OS)

- AKOT (OS)

ao

20

-20

Test Solution 2 at 120C 7m KCI + 1.8m NaNO3 + 1.2m NaCI + 2.4m Na2SO4

-100

1.0E-02


Ph

ase

An

gle

, deg

ree

4

: 41 . 0111

A ITK

AL" +X4X1 4 4■ XIO -

0 66 .4/' A g • -

ILI' -

.1X NIXX *.

RefX e-

-40 •

1XX22 11til izz " 430

+++++++,114;....--

•

OMPT- tl .... *M iStx x . e 41 40 ..•.

-100

1.0E-02 1.0E+05 1.0E-01 1.0E+00 1.0E+01 1.0E402

Frequency, Hz

1.0E+03 1.0E404

Ph

ase

An

gle

, d

eg

ree

so

ao

20

-2o


.1 1 Ar 2

A l "!

si I g •

0!• • A!. • 1

ei• • -

_ -

• .n Grade 23+Pd (FS)

• Ti Grade 29 (FS)

a Ti Grade 7 (FS)

+ AKOT (ES)


x Ti Grade 29 (OS)

• Ti Grade 7 (OS)

• AKOT (OS)

Test Solution 3 at 120C 7.2m KCI + 0.3m 10403 + 3.3m NaNO3 + 2.1m Na2SO4 + 0.2m NaF

i

-40 ttle g , 44

' es.xxxxxXxx_

** .

, ..

..... ■ $$... ** eco cl iii . 4 111"X * 40' 1

11* . 64 4 4 ' -

40 IMM,Vgifilififfig121,11,1111111filillifixiifilig ...

• • • • • • • 1 • •-_• •

1.0E+05 1.0E-01 1.0E+00 1.0E+01 1.0E+02

Frequency, Hz

1.0E+03 1.0E+04



60 -

40

20

0 4 1 eN

60 611 eg

A

co 0.8

a oi 0.6

3 0.4

a. • 0.2

2 r, • 0.0 tu

-0.2

-0.4

1.0E-09 1.0E-08 1.0E-07 1.0E-04 1.0E-03 1.0E-02


Phase

An

gle

, deg

ree


5m KC! + 2.8m KNO3 + 6.6m NaNO3 + 6.8m Na2SO4 + 0.1m NaF + 0.1m NaBr

• 11 Grade 23+Pd: Oxidized Surface

X 11 Grade 29: Oxidized Surface

• 11 Grade 7: Oxidized Surface


-20 -x

-40 • • ilt

_---- .

...+tilltz

Xxx...-

A pt + +x

-60 Xt - Ile + X

+++Auxi *****

i ++ xx x

I. ex ' o e +

114;:44:11144,11:114.111geM * ;ii

** 1.1.2.16! mmmmm .4!

• ••

44464* IIINC6 ***;//litt e l a l t4; 1 6"1"i" -80

-100

• 11 Grade 23+Pd: Fresh Surface




I T " e •

1.0E-02 1.0E-01 1.0E+00 1.0E+01 1.0E+02

Frequency, Hz

1.0E+03 1.0E+04 1.0E+05


1.2

Specimens: Fresh surface & followed by immersion for 28 days in aerated TS-1 solution + 7 days in dearated TS-1 solution at 150C. CPP Measurement was done in deaeared TS-1 solution at 150C

1.0

TS-1 Solution


1_01.

1.0E-06 1.0E-05

Current Density, A/cm2

Figure 46. Cyclic potentiodynamic polarization (CPP) curve for fresh (non-oxidized) Ti alloys in TS-1 at 150 °C. Note that no localized corrosion attack was observed after the CPP measurement.


1.2

1.0

TS-1 Solution


•••••

co 0.8 4

0.6

0.4

2

a. 0.2

a 0.0 tu

-0.2

1.0E-02 1.0E-03 1.0E-04 1.0E-09 1.0E-08 1.0E-07

0.8

AKO

Ti Grade 7

• • • • • •••• ro -4.1.1

Ti Grade 29

Ti Grade 23+Pd

". • j■ *41•••••■• 60••••

• • • •

•• •

TS-2 Solution

7m KCI + 1.8m NaNO3+1.2m NaCI+2.4Na2SO4

• i nitl 1. 11111“ II A A 11u, 1 1.111.11.1. 111.111, I LAL, -0.4

1.0E-06 1.0E-05


1.0E-09 1.0E-08 1.0E-07

Ele

ctr

od

e P

ote

nti

al,

V(A

g/A

gC

I)

0.6

0.4

0.2

1.0E-04 1.0E-03

0.0

-0.2


Specimens: Oxidized surface & followed by Immersion for 28 days

In aerated TS-1 solution + 7 days tn dearated TS-1 solution at 150C.

CPP Measurement was done in deaeared TS-1 solution at 150C

-0.4

1.0E-06 1.0E-05

Current Density, A/cm 2

Figure 47. Cyclic potentiodynamic polarization (CPP) curve for oxidized Ti alloys in TS-1 at 150 °C. Note that no localized corrosion attack was observed after the CPP measurement.

1.2

Specimens: Fresh surface & followed by immersion for 28 days

in aerated TS-2 solution + 7 days In dearated TS-2 solution at 120C.

CPP Measurement was done in deaeared TS-2 solution at 120C 1.0

1.0E-4



Ti Grade 29 AKO

Ti Grade 23+Pd

Specimens: Oxidized surface & followed by immersion for 28 days

in aerated TS-2 solution + 7 days in dearated TS-2 solution at 120C.


0.8

Ele

ctr

od

e P

ote

nti

al,

V(A

g/A

gC

I)

0.6

0.4

0.2

•••ot• ••• O •

• • • • • • 'JO 42'

TS-2 Solution

7m KCI + 1.8m NaNO3+1.2m NaCI+2.4Na2SO4

0.0

-0.2

1 I I I 11111 1 I 1 111, 11

1.0E-06 1.0E-05


1.0E-04 1.0E-03 1.0E-1

1 I I IL I I I 1 I I 1111,1

1.0E-08 1.0E-07

1.2

1.0

Ti Grade 7

-0.4

1.0E-09

Ti Grade 29

• a• ••• ••• • ••••' . ..

TS-3 Solution

7.2m KCI +0.3m KNO3 +3.3m NaNO3+2.1m Na2SO4+0.2m NaF 0.8

E.;

Ti Grade 23+Pd • • •.

qv•.• I • • • • • ••••••••••Ok

-0.2

••

•• • i• • • •

••• •

1. I I. .11 ■ 1111 -0.4

0.6

5;" To

*C 0.4

a.

lg. 0.2

(.)

LT,

0.0

Ti Grade 7

AKO

1.0E-1 1.0E-03 1.0E-04


Figure 49. Cyclic potentiodynamic polarization (CPP) curve for oxidized Ti alloys in TS-2 at

120 °C. Note that no localized corrosion attack was observed after the CPP measurement.

1.2

Specimens: Fresh surface & followed by immersion for 28 days

In aerated TS-3 solution + 7 days in dearated TS-3 solution at 120C.



Figure 50. Cyclic potentiodynamic polarization (CPP) curve for fresh (non-oxidized) Ti alloys in

TS-3 at 120 °C. Note that no localized corrosion attack was observed after the CPP measurement.

1.0

1.0E-07 1.0E-09 1.0E-08 1.0E-07 1.0E-06 1.0E-05


••••••

• • ••• • • IC •• V 4.124

Ti Grade 7

Ti Grade 29--o•

11 Grade 23+ Pd

AKO

• • • •••• • • • • • • • •

••• •••••• •II•ert, ACI.V:I• • •••••■• • :a a.. • •

TS-3 Solution

7.2m KCI +0.3m KNO3 +3.3m NaNO3+2.1m Na2SO4+0.2m NaF 11011,1 a Ill./LILL 1 1 11111111 1 -0.4

Ele

ctr

od

e P

ote

nti

al, V

(Ag

/Ag

CI)

1.2

1.0

0.8

0.6

0.4

0.2

0.0

-0.2

1.0E-09 1.0E-07 1.0E-08 1.0E-04 1.0E-03

Ele

ctr

od

e P

ote

nti

al,

V(v

s.

Ag

/Ag

CI)

1.2

1.0

0.8

0.6

0.4

0.2

0.0

-0.2

-0.4 LLL

1.0E-09 1.0E-07 1.0E-08 1.0E-04 1.0E-03


Specimens: Oxidized surface & followed by immersion for 28 days in aerated TS-3

solution + 7 days in dearatecl TS-3 solution at 120C.


1.0E-06 1.0E-05



1.0E-02

Specimens: Fresh surface & followed by Immersion for 28 days In aerated TS-4 solution + 8 days in dearated TS-4 solution at 150C

CPP Measurement was done In deaeared TS-4 solution at 150C

Ti Grade 23+Pd

11 Grade 7 • • •

• e••.9 .1.:

TS-4 Solution •

5m KCI + 2.8m KNO3 + 6.6m NaNO3 + 6.8m Na2SO4 + 0.1m NaF + 0.1m NaBr

1.0E-06 1.0E-05




gi 0.6

.7.2 0.4

2 o_

0.2

•m 0.0 uJ 0110 1

Ti Grade 23+Pd

Ti Grade 29

••••••••••• ■ • • • • •

TI Grade 7

AKOT

Y

_40°1+11

e"'"Ic e.001°-

-0.4

1.0E-07 1.0E-09 1.0E-08


1.2

1.0

Specimens: Oxidized surface & followed by immersion for 28 days

in aerated TS-4 solution + 8 days in dearated TS-4 solution at 150C


o 0.8 psof'

•■••• -0.2 TS-4 Solution

5m KCI + 2.8m KNO3 + 6.6m NaNO3 + 6.8m Na2SO4 + 0.1m NaF + 0.1m NaBr

1111•. 1 • I. I 1.•11

1.0E-02 1.0E-06 1.0E-05



1.0E-04 1.0E-03


OFFICE OF CIVILIAN RADIOACTIVE WASTE MANAGEMENT 1. OA: OA

SPECIAL INSTRUCTION SHEET Page 1 of 1

This is a placeholder page for records that cannot be scanned.

2. Record Date 3. Accession Number

10/02/06 TD'. HOL .)ba(A 1 oq.0010 4. Author Name(s) 5. Authorization Organization

P.L. Andresen, Y.J. Kim Lead Lab/PA

_ 6. Title/Description 5t- re_s5 Ckly row^. Crac..4 lnitict-i-o-W■ 4 Girou-l-vk

Attachment to GE GRC Final Report No. GE-GRC-Bechtel-2006-2. rYIR -re-In P-fki.S i 4 EAVIbrOil 11-‘24‘43 Fe 1 a-va4.4- i -b th 3 h Le tie_A 14m but."( 6-)113%e_ P4c.344,512 S

et.c,A4,ac,hvvvixt.4. 7. Document Number(s) 0 ,00-1 8. Version Designator

GE-GRC -Bechtel -2006-2 N/A

9. Document Type 10. Medium

Report CD Ci)

11. Access Control Code

12. Traceability Designator

GE-GRC-Bechtel-2006-2

13. Comments

SOFTWARE - text editor, WinZip, Excel, Adobe

See attached file listing

, ,

XREF MOL.20061108.0004 THIS IS AN ELECTRONIC

ATTACHMENT

NOV 0 9 2006 .-77544,,c4

MD5 Validation

FORM NO. A171-1 (Rev. 11/23/2005) AP-17.1Q

\AlijaAAA-WA- b.c WA-- fra.rxie...te

.r.L--• YVL,A.,•U.4..0,`-s--

1111-106

dir.txt Volume in drive D is New Volume Serial Number is D530-7C66

Directory of D:\

10/06/2006 10/02/2006 10/02/2006 10/19/2006 10/19/2006 10/02/2006 10/06/2006 10/17/2006 10/02/2006 10/06/2006

12:11p <DIR> Crack Growth Rate

05:23a <DIR> Cyclic Potentiodynamic Polarization Data

05:23a <DIR> Electrochemical Impedance Data

03:30a 2,598,400 GE-GRC-Final-Sept-2006-Rev3.doc

03:37a 2,747,099 GE-GRC-Final-Sept-2006-Rev3.pdf

05:23a <DIR> H2 Measurement

12:18p <DIR> Keno

10:34a <DIR> Lab Notebooks

05:23a <DIR> Open-Circuit Potential Data

12:18p <DIR> Ti-Air-Data 2 File(s) 5,345,499 bytes

Directory of DACrack Growth Rate

10/06/2006 10/06/2006 03/03/2001 07/17/2005 05/12/2000 07/19/2005 10/06/2006 10/06/2006 10/06/2006 10/06/2006 10/06/2006 10/06/2006 10/06/2006 10/06/2006 10/06/2006 10/06/2006 10/06/2006 10/24/2000 01/16/2002 02/03/2004 02/03/2004 02/03/2004 09/30/2006 09/30/2006 09/30/2006 09/30/2006 09/22/2005 09/22/2005 10/11/2006 10/11/2006

<DIR> <DIR>

12:11p 12:09p 03:40p 05:15a 03:50a 05:28p 06:09a 10:53a 10:56a 11:00a 11:03a 11:11a 11:13a 11:32a 11:36a 11:44a 11:43a 10:43a 06:48p 04:53p 05:31p 05:52p 10:17a 10:21a 10:47a 02:43p 05:51a 05:49a 06:41p 06:41p

28 File(s)

3,099,648 a44LLNL.xLS 13,828 COMMENTS.143 11,397 COMMENTS. 144 17,426 COMMENTS.148 17,266 COMMENTS.152 23,853 COMMENTS.153 40,298 COMMENTS.200 12,940 COMMENTS.263 12,940 CommENTs.264 27,857 COMMENTS.265 21,994 COMMENTS.266 7,408 COMMENTS.268 7,408 COMMENTS. 269

83,913 COMMENTS.287 64,894 COMMENTS.288

3,438,592 c14311n1.xls 8,457,728 c148.xls 16,920,576 c152.xls 14,479,360 c153.xls 5,246,464 c200.xls

10,681,856 c263.xls 9,483,264 c264.xls 11,452,928 c265.xls 10,140,672 c266.xls 4,497,408 c268.xls 4,014,080 c269.xls 5,918,720 c287.xls 3,436,544 c288.xls

111,631,262 bytes

Directory of D:\Cyclic Potentiodynamic Polarization Data

10/02/2006 10/06/2006 09/11/2006 09/26/2006 09/26/2006 09/11/2006

05:23a <DIR> .

12:09p <DIR> ..

03:45a 2,265,600 Cyclic PP, TS1.xls

12:23p 2,173,952 Cyclic PP, TS2.xls

12:27p 2,121,728 cyclic PP, TS3.xls

03:45a 2,023,424 Cyclic PP, TS4.xls 4 File(s) 8,584,704 bytes

Directory of D:\Electrochemical Impedance Data

Page 1

10/02/2006 10/06/2006 07/19/2006 08/08/2006 08/08/2006 07/19/2006

dir.txt

05:23a <DIR> •

12:09p <DIR> ..

12:25p 332,288 EIS-TS1.xls

05:38a 278,016 EIS-TS2.xls

09:10a 278,528 EIS-TS3.xls

12:24p 327,680 EIS-T54.xls 4 File(s) 1,216,512 bytes

Directory of D:\H2 Measurement

10/02/2006 10/06/2006 06/21/2006 08/14/2006

05:23a 12:09p 02:48a 10:08a

2 File(s)

<DIR> . <DIR> ..

154,772 H2 Content-GEC0010606174450011.pdf 248,461 H2 Content-GEC0010608224541.pdf 403,233 bytes

Directory of D:\Keno

10/06/2006 12:18p <DIR> .

10/06/2006 12:09p <DIR> ..

10/17/2006 08:50a 137,216 ttf-plot-10-02-06.xls 1 File(s) 137,216 bytes

Directory of D:\Lab Notebooks

10/17/2006 10/06/2006 10/16/2006 10/17/2006 10/16/2006 10/16/2006 10/16/2006 10/16/2006 10/17/2006

10:34a <DIR> .

12:09p <DIR> ..

02:10p 544,968 Lab-Notebook-CT_string.pdf

04:45a 2,355,290 Lab-Notebook-Creep-U-Bend.pdf

01:51p 2,509,936 Lab-Notebook-Kim.pdf

02:02p 2,097,631 Lab-Notebook-SCC_39SE.pdf

02:04p 2,144,113 Lab-Notebook-SCC_47A1.pdf

02:05p 1,723,217 Lab-Notebook-SCC_47A2.pdf

05:11a 8,212,475 Lab-Notebook-SCC_Keno.pdf 7 File(s) 19,587,630 bytes

Directory of D:\Open-Circuit Potential Data

10/02/2006 05:23a <DIR> .

10/06/2006 12:09p <DIR>

09/26/2006 12:57p 388,608 OCP Data,.xls 1 File(s) 388,608 bytes

Directory of D:\Ti-Air-Data

10/06/2006 12:18p 10/06/2006 12:09p 04/07/2005 05:51a 04/17/2005 01:59a 12/01/2005 04:19a 12/01/2005 04:19a 12/01/2005 04:19a 12/01/2005 04:19a 06/30/2006 12:16p 03/28/2005 02:18p 08/31/2005 01:15p 04/19/2005 10:11a 04/19/2005 10:11a 04/19/2005 10:11a 10/01/2006 10:12a 10/18/2006 09:43a 10/01/2006 10:13a 10/18/2006 09:44a

<mil> . <DIR> ..

7,238,656 TIARQAC4.xls 2,457,600 TIARQAC4a.xls 2,025,984 TIARQAC4b.xls 2,919,424 TIARQACreep1P1ot.xls

116,736 TIARQACreep2P10t.xls 429,568 TIARQACreep3P10t.xls 167,424 TIARQACreep4P1ot.xls 44,032 TIARQATensilel Plot.xls 35,328 TIARQATensile2Plot.xls 19,456 Ti 2 vs Ti 5 creep rate vs stress.xls 19,968 Ti Creep Rate vs Stress.xls 20,992 Ti Creep Strain vs Stress.xls

156,672 Ti7C5-Yield-Strength.xls 2,001,920 Ti7C6-Yield-Strength.xls 859,136 Ti7c5-Creep5-Plot.xls 293,888 TiGr29C1 Plot.xls

Page 2

dir.txt

16 File(s) 18,806,784 bytes

Total Files Listed: 65 File(s) 24 oir(s)

166,101,448 bytes 0 bytes free

Page 3

stress corrosion crack initiation & growth measurements in ...final report prepared under...

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