Publications (YM) Yucca Mountain 1-18-2007 Sub-surface corrosion research on rock bolt system, perforated Sub-surface corrosion research on rock bolt system, perforated SS sheets and steel sets for Yucca Mountain Repository SS sheets and steel sets for Yucca Mountain Repository Dhanesh Chandra University of Nevada, Reno, [email protected]Jaak J.K. Daemen University of Nevada, Reno, [email protected]Follow this and additional works at: https://digitalscholarship.unlv.edu/yucca_mtn_pubs Part of the Civil and Environmental Engineering Commons, and the Metallurgy Commons Repository Citation Repository Citation Chandra, D., Daemen, J. J. (2007). Sub-surface corrosion research on rock bolt system, perforated SS sheets and steel sets for Yucca Mountain Repository. Available at: Available at: https://digitalscholarship.unlv.edu/yucca_mtn_pubs/12 This Presentation is protected by copyright and/or related rights. It has been brought to you by Digital Scholarship@UNLV with permission from the rights-holder(s). You are free to use this Presentation in any way that is permitted by the copyright and related rights legislation that applies to your use. For other uses you need to obtain permission from the rights-holder(s) directly, unless additional rights are indicated by a Creative Commons license in the record and/or on the work itself. This Presentation has been accepted for inclusion in Publications (YM) by an authorized administrator of Digital Scholarship@UNLV. For more information, please contact [email protected].
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Publications (YM) Yucca Mountain
1-18-2007
Sub-surface corrosion research on rock bolt system, perforated Sub-surface corrosion research on rock bolt system, perforated
SS sheets and steel sets for Yucca Mountain Repository SS sheets and steel sets for Yucca Mountain Repository
Follow this and additional works at: https://digitalscholarship.unlv.edu/yucca_mtn_pubs
Part of the Civil and Environmental Engineering Commons, and the Metallurgy Commons
Repository Citation Repository Citation Chandra, D., Daemen, J. J. (2007). Sub-surface corrosion research on rock bolt system, perforated SS sheets and steel sets for Yucca Mountain Repository. Available at:Available at: https://digitalscholarship.unlv.edu/yucca_mtn_pubs/12
This Presentation is protected by copyright and/or related rights. It has been brought to you by Digital Scholarship@UNLV with permission from the rights-holder(s). You are free to use this Presentation in any way that is permitted by the copyright and related rights legislation that applies to your use. For other uses you need to obtain permission from the rights-holder(s) directly, unless additional rights are indicated by a Creative Commons license in the record and/or on the work itself. This Presentation has been accepted for inclusion in Publications (YM) by an authorized administrator of Digital Scholarship@UNLV. For more information, please contact [email protected].
YM –DOE Review Meeting At DRI, Reno January 18, 2006 (1 – 1.25 pm)
Dhanesh Chandra* - PIJaak Daemen** - Co-PIRaul B. Rebak***- National Laboratory Collaborator (LLNL)Michael Mohorich*- MS Graduate Student Anjali Talekar*- Ph.D Graduate StudentSuresh Divi*- Ph.D Graduate StudentJosh Lamb*- Ph.D Graduate Student*Metallurgical & Materials Engineering, University of Nevada, Reno 89557**Mining Engineering, University of Nevada, Reno 89557***Lawrence Livermore National Laboratory, Livermore CA 94551
Sub-surface Corrosion research on Rock Bolt system, Perforated SS Sheets and
Steel Sets for Yucca Mountain Repository
- Presented to -
YM Project Program Review Panel Members
YM-DOE Program Review -DRI, Reno 1-18-07
• Metallurgical Issues in Underground Repository Reinforcement Support for Nuclear Materials Storage in simulated Yucca Mountain Environment used for Corrosion Issues
• Issues related to I-beams (Low Carbon) and Rock Bolts (Med. Carbon)
• Experimental
• Results
1. Corrosion Tests- Effect of Ionic Concentration (1x,10x,100x), Temperature, concentration and aeration/deaeration effects in YMwaters (RB and I-Beam)
2. Hydrogen Permeation Tests
3. Environmentally Assisted Corrosion Tests - Stress Corrosion Cracking/Hydrogen Embrittlement in 100x YM water concentration at Room Temperature and 85oC (I-Beams)
Subsurface Facilities Criterion:a)thermal-mechanical stressesb)loads from constructionc)loads from repository operationsd)in situ loads from the overlying rocks e)loads from seismic occurances
Emplacement tunnels:• 18ft diameter• 52 required to emplace 70,000 metric tons• 35 miles total length
• Rock bolts will be installed for structural integrity of the tunnel
• Typical rock bolt for this application is 10 ft long
YM - Subsurface Design
Friction Rock Bolt
YM-DOE Program Review -DRI, Reno 1-18-07
Rockbolts
I-Beam
Rock Bolt and Steel Sets in Yucca Mountain (YM) Environment
Waste Packages
Objective of Study:Determine Corrosion Rates Aerated/Deaerated
Simulated Environment Stress Corrosion Cracking Effects and Hydrogen
embrittlement Behavior in YM Nuclear Repository
Background
Tubular
Solid - w/small diameter hole
YM-DOE Program Review -DRI, Reno 1-18-07
Summary of Task ORD-FY04-019
In ProgressStress corrosion cracking (SCC) research
(Major Task to be started)
Task 2Task 2
CompletedFor Rock bolts
Electrochemical Corrosion (Polarization and Impedance)
studies
Task B1(Additional Task of
Impedance Spectroscopy was
carried out at UNR in this task)
In progress for rock bolts and steel
Salt Spray MethodTaskA1 (1.4)
CompletedFor rock bolts
Aqueous CorrosionTaskA1 (1.3)
In ProgressFor rock bolts
Humid Air CorrosionTaskA1 (1.2)
In ProgressDry OxidationTaskA1 (1.1)Task 1
StatusTaskSIP Task No.
YM-DOE Program Review -DRI, Reno 1-18-07
Tasks (Cont’d)
Completed for Rock bolts and more work is
in progress.
X-ray Photoelectron Spectroscopy (XPS)
Task 3.3 (Additional task carried out to study the oxide film formed, this task is not mentioned in SIP)
Completed for Rock bolts and further work
is in Progress
Scanning Electron Microscopy and Energy Dispersive analysis (SEM-
EDX)
Task 3.3
Needs to be done. Scoping studies
already performed
Atomic Force Microscopy (AFM)Task 3.3
Majority work done, in a process of
completion for steel sets
Hydrogen Permeation ResearchTask 3.2
Hydrogen Embrittlement (HE) Research
Task 3.1\
YM-DOE Program Review -DRI, Reno 1-18-07
Materials and Methods Used for Sub-surface Reinforcing Corrosion Study
Materials
Rock Bolts
Williams Hollow Core MC Steel
(From YM Site)
Split Sets (HSLA)
Swellex Rock Bolts (HSLA)
CT Rock Bolts
Sub-Surface Support Liners
Steel Sets (I-Beam from YM Site )
Bernold Shields (4340 Steels)
Other Alloys
Alloy 22 (Ni Base Alloys)
Methodologies Used to Determine Corrosion rates and other
Properties1. Potentiodynamic Method
2. Potentiostatic Method
3. Electrochemical Impedance Studies
4. Immersion Studies
(ASTM G-31)
5. Cyclic Humidity Studies (ASTM-G-60)
6. Water Spray test (Modified Water Spray G-85 tests)
LONG-TERM TES TS (Fille d S ymbols) YMWS = YM Wa t e r S pra y (1x)CH= Cyc lic Humidit y (1x)P I= P a rt ia lly Imme rse d (1x)NI= Non Imme rse d (1x)CI= Comple t e ly Imme rse d (1x)
Nitrogenated
Oxygenated
Oxy
gena
ted
Rock Bolts (0.44%C)
YM-DOE Program Review -DRI, Reno 1-18-07
Temperature Effects on CR of Rock Bolts (0.44%C) in Aerated (Oxygenated) YM waters
0
200
400
600
800
1000
1200
20 30 40 50 60 70 80 90
Temperature (degree of celcius)
Cor
rosi
on R
ate
(mic
ron/
year
)
1X10X100X
Ix and 10x YM waters → Similar Behavior
100x → Different Behavior with a Maxima at~45oC
Corrosion Rates vs Temperature in AERATED YM Waters
Potentiodynamic Polarization of aerated 1x YM Water
-1-0.9-0.8-0.7-0.6-0.5
-0.4-0.3-0.2-0.1
0
1.E-07 1.E-06 1.E-05 1.E-04 1.E-03 1.E-02 1.E-01
Current Density(A/cm2)
Pote
ntia
l(V);v
s Ag
/AgC
85oC
25oC1X YM Water
Tem.Eff in 100xo
-1
-0.8
-0.6
-0.4
-0.2
0
0.2
1.E-08 1.E-06 1.E-04 1.E-02 1.E+00
Curent Density(A/cm2)
Pote
ntia
l(V)
25456585
Rock Bolt Potentiodynamic Scans Showing Temperature Effect on Icorr
45oC
100X YM Water
-1.0
-0.9
-0.8
-0.7
-0.6
-0.5
-0.4
1.0E-09 1.0E-07 1.0E-05 1.0E-03
Current Density (A/cm2)
Appl
ied
Pote
ntia
l (V)
25oC
85oC
75oC
45oC
90oC
YM-DOE Program Review -DRI, Reno 1-18-07
I-Beam-Baseline Studies Potentiostatic and Dynamic Test
0.00E+00
2.00E-07
4.00E-07
6.00E-07
8.00E-07
1.00E-06
1.20E-06
0 10000 20000 30000 40000 50000 60000 70000 80000
Time (sec)
Perm
eati
on C
urre
nt (I
p, a
mp/
cm2 ) HCO3
- SiO32-
HCO3- +SiO3
2-
Baseline scan
Potentiodynamic Curves in water (0% NaCl) (A) With no extra added Ions (B) 0.01 M SiO3
2- (C) 0.5 M HCO3-, (D)
0.01 M SiO32- + 0.5 M HCO3
-
Silicate Ions do not play any role in passivation when present with Bicarbonate ion in Plain DI water
Example of Swellex Mn 24-Immersion test-25oC-Corrosion Rates
YM-DOE Program Review -DRI, Reno 1-18-07
0.955
0.96
0.965
0.97
0.975
0.98
0.985
0.99
0.995
1
1.005
0 1 2 3 4 5 6 7 8Time(days)
Mas
s(g)
Rockbolt
Steel set
0.994
0.995
0.996
0.997
0.998
0.999
1
1.001
0 5 10 15 20 25
Time(Days)
Mas
s(g)
Rock Bolt
Steel Set
Salt Spray and Humidity tests of Rock Bolt and I-Beam
Salt spray Fog Tests
Weight Loss
Humidity Chamber
Weight Loss
I beam corrosion rates are lower than that of rock-bolt in both in spray (Fog) conditions and Humid Environments of 1xYM water. The CR difference is higher in salt spray tests due to
the concentration cell effects.
I-Beam CR ~19 μm/yr
RB CR ~45 μm/yr
I-Beam CR ~910 μm/yr
RB CR ~800 μm/yr
YM-DOE Program Review -DRI, Reno 1-18-07
“Static” - Strain Aging Phenomenon
Recovery of Yield Point due to Aging for a long time (months) to create Cottrell atmospheres.
This process can be accelerated with Temperature as it controls diffusion of atoms ( In Steels usually T < 400oC recovery is observed)
Cottrell – Bilby
f = Solute segregated to a Dislocation in time t
f = α. ρ.(A.D.t / kT)2/3
A= Interaction constant
D= Diffusion Coeeficient
ρ = Total Length of dislocation /unit volume
Harper
f = Solute segregated to a Dislocation in time t
f = 1- exp [α. ρ.(A.D.t / kT)2/3]
Stre
ss
Strain Strain
Strain Aging
• When Aging Occurs During deformation, the phenomenon is termed Dynamic Starinaging
• Dynamic Strain aging work hardening rate is abnormally high and also dependent on the Temperature and Strain rate.
• Increasing Temperature also increases the maximum work hardening
Dynamic Strain Aging Phenomenon
YM-DOE Program Review -DRI, Reno 1-18-07
100xn85 Ecorr
0
100
200
300
400
500
600
700
800
0 1 2 3 4 5
Position(m m )
Load
(kg)
I-Beam (100xYM Water) at 85oC and at Ecorr
Lüder Bands
285
295
305
315
325
335
345
355
0.3 0.4 0.5 0.6 0.7Elongation(mm)
Load
(kg)
A
630
640
650
660
670
680
690
700
710
3.8 4 4.2 4.4Elongation(mm)
Load
(kg)
B
Dynamic Strain Aging (DSA) Occurred At 85°C at Ecorr Open Circuit Potential Portevin LeChatelier Effect
I-Beam in 100x YM water at Ecorr
-0.8
-0.6
-0.4
-0.2
0
Pote
ntia
l (V)
; vs
Ag/A
gCl
Ecorr
Plastic flow tends to become unstable leading to serrations
YM-DOE Program Review -DRI, Reno 1-18-07
0
100
200
300
400
500
600
700
0 0.05 0.1 0.15 0.2 0.25Strain
Stre
ss (
MPa
)
85oC(+50 mV)I-Beam (100x YM waters)
25oC(+50 mV)
Stress Strain Curves of I-Beams At RT and 85 °C
25°C Ductile Failure with Secondary
Cracks85 °C Brittle
Failure
Dynamic Strain Aging (DSA) Occurred At 85°C at -650 mV (Ecorr~-700mV)
Portevin LeChatelier Effect
25 °C 85 °C
85oC (-650 mV)
25oC (-650 mV)
YM-DOE Program Review -DRI, Reno 1-18-07
300
350
400
450
500
550
600
650
0 0.05 0.1 0.15 0.2 0.25Strain
Stre
ss(M
Pa)
MechanicalTest
-600 mVEcorr
-750 mV
-900 mV
-1200 mV
-650 mV
SSRT Behavior of I-Beam At Various Potentials in
100x YM Water
Ecorr -700mV
85 °C
YM-DOE Program Review -DRI, Reno 1-18-07
250
300
350
400
450
500
550
0 0.05 0.1 0.15 0.2 0.25
Strain
Stre
ss(M
Pa)
Glycerine
-750-1200
-700 (Ecorr)
-900 -650-600
Inert environment
Effect of High Cathodic Charging in
100x YM Waters
Room Temperature Scans at Various Potentials Showing No Dynamic StrainAging Effects on the Low Carbon Steel in 100x YM Deaerated Waters
Room Temperature
YM-DOE Program Review -DRI, Reno 1-18-07
0
100
200
300
400
500
600
700
0 0.05 0.1 0.15 0.2 0.25 0.3Strain
Stre
ss(M
Pa)
25 oC
85 oC
Areas which are the measure of ductilities at 25 oC and 85 oC
Figure 4c.12. Ductility differences of LCS revealed by mechanical tests at RT and 85 oC in air with the strain rate 10-6/s . The difference in the rectangular surface areas as a measure of ductility shows the increased embrittlement in the steel due to strain aging, or PLC effect.
Metallurgical and Materials Engineering University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
-6.E-04
-5.E-04
-4.E-04
-3.E-04
-2.E-04
-1.E-04
0.E+00
1.E-04
2.E-04
0 20000 40000 60000 80000 100000 120000Time(s)
Cur
rent
(A)
-0.0077
-0.0067
-0.0057
-0.0047
-0.0037
-0.0027
-0.0017
-0.0007
0.0003
Cur
rent
(A)
-600 mV
-650 mV
- 700 mV
-750mV
-900 mV
-1200 mV (refer to right hand side axis)
-600
-650
-750-900
-1200
25°C
-5.0E-05
-4.0E-05
-3.0E-05
-2.0E-05
-1.0E-05
0.0E+00
1.0E-05
2.0E-05
0 20000 40000 60000 80000 100000 120000
Time(s)
Cur
rent
(A)
-650 mV
-600 mV-700 mV
-750 mV
These two curves are referred to the right hand side axis
Correlated Ecorr change with the serration amplitudes of PLC effect in Low Carbon Steel during SSRT in YW water caused a large amount of potential change at the interface of LCS and the Test Solution.
Plots of Load vs Elongation and Ecorr vs Time (sec) during a SSRT A Test in YW water at the Constant Strain Rate of 1.6x10-6/s
Potential
85oC
50oC 55oC65oC
85oC
Specimen Failure
Load
1.3 1.8 2.3 2.8 3.3 3.8 mm
600
620
640
660
680
700
720
740
1.3 1.8 2.3 2.8Elo ngat io n(mm)
Load vs Elongation Curve
Elongation
70oC
YM-DOE Program Review -DRI, Reno 1-18-07
10
20
30
40
50
60
70
80
1.0E-07 1.0E-06 1.0E-05 1.0E-04 1.0E-03 1.0E-02
Strain Rate(1/s)
Red
uctio
n of
Are
a(%
)
85 oC
25 oC
Embrittlement by Strain Aging and Hydrogen
Stress Corrosion Cracking
Measure of Ductility by R of A Obtained At Various Slow Strain Rates Ranging From 10-3/s to 10-7/s at 25oC and 85oC
for I-Beam Supports at Ecorr -700 mV
Metallurgical and Materials Engineering, University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
General Cracking Modes of I-Beam (1.6x10-7/sec) 25 °C, Air
Ductile Failure85°C Elec-Mech
Inner Longitudinal
Cracks
Load
Load
T G
I G
T G
I G
25°C Elec-Mech.
Secondary Cracks
25oC (@Ecorr = *-700mV)
25oC (*Potential -900oC)
*Potential Reference Ag/AgCl Electrode
YM-DOE Program Review -DRI, Reno 1-18-07
Fracture Morphology of I-Beam at 25°C and 85 °C
Metallurgical and Materials Engineering University of Nevada, Reno Results
Ductile FailureSSRT Air - 25 °C
Quasi cleavage-slip Mode
SSRT 85°C 100xYM Waters
Transgranular Cracks
The ridges are due to PLC effect. Average length ~0.4 mm
Measure of ductility by Reduction of Area values of I-Beam Under
various specimen Potentials at Room Temperature and 85oC
Measure of Ductility of I-Beam Under Various Specimen Potentials at Room temperature and 85 oC
Measure of ductility by % Elongation of LCS under various
specimen potentials at Room Temperature and 85oC
Metallurgical and Materials Engineering, University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
OXIDATION KINETIC STUDIES OF ROCK BOLTS
nWy ktA
⎛ ⎞⎜ ⎟⎝ ⎠
= =Oxidation Rate Law: (W/A) is the weight gain per unit area at time t,
k is the rate constant, and
n is the time exponent of the rate law.
Isothermal and non-isothermal kinetics can be given by:
)().( αα fTkdtdr ==
α is the extent of reaction,
k(T) is the temperature dependent rate constant (a constant value for isothermal experiments)
0 expaEk k
RT⎛ ⎞−Δ
= ⎜ ⎟⎝ ⎠
The rate constant follows an Arrhenius expression
( )0( ) sin 2avg TT t T t A t Pβ π= + + ⋅
Temperature profile in a typical modulated thermogravimetric analysis:
βavg = underlying heating rate = 0 (isothermal)
( )sin 2TA t Pπ ⋅ (A time varying perturbation to the isothermal T0temperature )
YM-DOE Program Review -DRI, Reno 1-18-07
2.22 x 10-4
2.67 x 10-40.7709
0.7900
7.122 x 10-5
6.5 x 10-50.7013
0.7825
9.27 x 10-5
6.24 x 10-50.6685
0.7750
0.41775.04
1.60 x 10-5
4.05 x 10-50.7859
0.7675
Mn-24
9.35 x 10-4a
2.71 x 10-40.5828a
0.7900
2.3212 x 10-4
1.433 x 10-40.7302
0.7825 3.693b92.81b
2.44 x 10-5
6.72 x 10-50.7968
0.7750SS-46
ko(kg2m-
4s-0.7)
Activation energy
(kJ/mol)b
Rate constant (k)(kg.m-2s-n)a
Index of Rate
Law (n)
T(oC)
Material
Time constants (n), Rate constants (k), activation energies and pre-exponential factors (k0) for the HSLA steels in the first oxidation regime.
YM-DOE Program Review -DRI, Reno 1-18-07
SUMMARY
Effect of Temperature Under Electrochemical EnvironmentDynamic Strain Aging Effects (Portevin Le Chatelier Effect) occurs at ~70°C contributing to significant embrittlement under YM simulated repository environmentsCorrosion rates of Rock bolts and I-beams
Hydrogen Permeation
Oxidation Studies
Salt Spray and Immersion Tests
Future Studies
•Mechanistic –XPS Studies
•Stress Corrosion Cracking further
•Oxidation Kinetic Studies
•Potentiodynamic and Potentiostatic studies
YM-DOE Program Review -DRI, Reno 1-18-07
Thank you
Metallurgical and Materials Engineering University of Nevada, Reno
We Thank YM US DOE for Support of this Project
We also thank DOE Program Managers and HRC Directors and QA staff for their Cooperation and Help on the project
YM-DOE Program Review -DRI, Reno 1-18-07
YM Water (Salt) Spray Tests
Specimens shown after 48 hour exposure
period.
After
C.Rate = ____________K x WA x T x D
The corrosion rates have been determined from the weight loss measurements of rock bolt and I-beam coupon specimens for 35oC.
Rate of Rock Bolt: 814 μm/year
Rate of I-Beam: 970 μm/year
CR values are close to the Partial immersion values. Coupon surfaces in this case were exposed to YM water partially too, during the entire fog type exposure time.
Before
Rock Bolt Specimens
I-Beam
YM-DOE Program Review -DRI, Reno 1-18-07
Figure 3.1.2 Potentiodynamic scans for SS46 type rock bolts in aerated simulated 1x YM water at different temperatures.
Figure 3.1.3. Corrosion rate as a function of temperature (aerated) in 1x YM water.
The films formed in the aerated YM waters are different in nature with compared to the deaerated ones; They are not see through, thick and softer.
Etched outrock bolt
Metal
Surface Film Formation and Pitting in 100x YM waters at 85oC
Results
Metallurgical and Materials Engineering University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
Precipitate layers formed on I-Beam at 25°C in 100x YM waters at RT. The scale peals of easily when they meet dry air after taken out of the cell. However the high temperature films are non porous and see through.
85°CRT
YM-DOE Program Review -DRI, Reno 1-18-07
The precipitate layer at 25 °C,
Porous scale lets EDX electrons to enter Fe
underneath
Mostly chloride and oxide scales with less
solubility at Low temperatures
The precipitate layer at 85°C,
Nonporous and more protective layer
Possible Silicon oxide or magnesium chloride
Mn and Fe absence
Scale differences at RT and 85°C on I-Beam Tensile Specimen
YM-DOE Program Review -DRI, Reno 1-18-07
25 oC 85 oC
Metallurgical and Materials Engineering University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
SUMMARY (Cont’d)
Environmentally Assisted Cracking of I-Beams (0.08%C)
100x YM waters
I-Beams are susceptible to SCC at 25°CEffect of Temperature Under Electrochemical Environment•Dynamic Strain Aging Effects (Portevin Le Chatelier Effect) occurs at ~70°C contributing to significant embrittlement under YM simulated repository environments
Isothermal Tests
High Temperature (85oC)
•Dynamic Strain Aging Effects occur at electrochemical potentials in I-Beams
•Hydrogen Induced Cracking occurs at the cathodic interface potentials; and also hydrogen blistering
Room Temperature•Stress Corrosion Cracking occurs under applied potentials in I-Beams
Metallurgical and Materials Engineering University of Nevada, Reno
YM-DOE Program Review -DRI, Reno 1-18-07
Repeatability test of the Set-Up with SS 304 in NaOH
Repeatibility tests are the preliminary experiments which should be done to make sure the results are able to be produced with in acceptable accuracy range. In our case it is less than 20 mV voltage change range which is well accepted by the ASTM Stardards.
Metallurgical and Materials Engineering University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
Summary of the Rates (micron/year)Electrochemical RB (Deaerated) Immersion RB (1x) YM Water
spray (1x)
1x
10x
100x
25oC 45oC 65oC 85oC
35 55 110 160
50 65 109 162
45 62 107 159
Electrochemical (Aerated)
1x
10x
100x
25oC 45oC 65oC 85oC
100 250 550 1100
101 300 710 1050
210 480 220 150
75oC200
513
960
fully
Hum.air
partially
35oC
814
970
RB
I-Beam
Aer
ated
Aer
ated
ambi
ent
Aer
ated
Humidity Chamber
19
45
Dea
erat
ed
RB
SS
25oC 75oC
45 200
Metallurgical and Materials Engineering University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
Taken out before the pitting potentials. Deaerated 65oC YM water. Shows protective film formation over the surface
Continued scan over the pitting potentials, and observed pitting
Surface Films Formed on Rockbolts in Deaerated Waters
Results
Metallurgical and Materials Engineering University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
Deaerated
Film formations specimens YM Waters
Inclusions
Metallurgical and Materials Engineering University of Nevada, Reno Results
Aerated
White Precipitate
YM-DOE Program Review -DRI, Reno 1-18-07
Polarization plots of I beam samples in Nitrogenated 100x solution
-1.2-1
-0.8-0.6-0.4-0.2
0
-8 -6 -4 -2 0
Log (i) A/cm2
Ecor
r (V
) vs
Ag/
AgC
l
25oC (Blue)
45oC (Purple)
85oC (Brown)
65oC (Dark Green)
-6 -4 -2 0
log (i) A/cm2
25oC (Blue)
45oC (Purple)85oC (Brown)
65oC (Dark Green)
Polarization plots of I beam samples in Oxygenated 100x solution
-1-0.8-0.6-0.4-0.2
00.2
-8 -6 -4 -2 0
Log (i) A/cm2Ec
orr(
V) v
s A
g/A
gCl
25oC (Blue)
45oC (Purple)
85oC (Brown)
65oC (Dark Green)
Metallurgical and Materials Engineering University of Nevada, Reno Results
Polarization Plots of I-Beam in 1x Oxygenated Solution
YM-DOE Program Review -DRI, Reno 1-18-07
100xn85 Ecorr
0
100
200
300
400
500
600
700
800
0 1 2 3 4 5
Position(mm)
Load
(kg)
I-Beam (100xYM Water) at 85oC and at Ecorr
Lüder Bands
0
100
200
300
400
500
600
700
0 0.05 0.1 0.15 0.2 0.25Strain
Stre
ss (
MPa
)
85oC(+50 mV)I-Beam (100x YM waters)
25oC(+50 mV)
Metallurgical and Materials Engineering University of Nevada, Reno Results
Lüder Band and Dynamic Strain Aging Effect at 85 °C
I-Beam in 100x YM water at Ecorr
Open circuit Potential Portevin LeChatilierEffect
YM-DOE Program Review -DRI, Reno 1-18-07
Polarization Plots of I-Beam in YM 1x Solution
Polarization plots of I beam samples in Nitrogenated 100x solution
-1.2-1
-0.8-0.6-0.4-0.2
0
-8 -6 -4 -2 0
Log (i) A/cm2
Ecor
r (V
) vs
Ag/
AgC
l
25oC (Blue)
45oC (Purple)
85oC (Brown)
65oC (Dark Green)
Polarization plots of I beam in 1x nitrogenated solution
-1.2-1
-0.8-0.6
-0.4-0.2
0
-8 -6 -4 -2 0
log (i) A/cm2
Ecor
r (V
) vs
Ag/
AgC
l
25oC (Blue)
45oC (Purple)
85oC (Brown)
65oC (Dark Green)
Metallurgical and Materials Engineering University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
-1
-0.8
-0.6
-0.4
-0.2
0
0.2
-8 -6 -4 -2 0
log (i) A/cm2Ec
orr
(V) v
s A
g/A
gcl
Polarization plots of I beam samples in Oxygenated 100x solution
-1-0.8-0.6-0.4-0.2
00.2
-8 -6 -4 -2 0
Log (i) A/cm2
Ecor
r(V
) vs
Ag/
AgC
l
25oC (Blue)
45oC (Purple)85oC (Brown)
65oC (Dark Green)
igure 2. Polarization plots of steel set samples measured in YM water under deaerated conditions at different temperatures. (top left) 1x (bottom left)1
igure 3. Polarization plots of steel set samples measured in YM water under aerated conditions at different temperatures. (Top right A) 1x (Bottom Ri
Metallurgical and Materials Engineering University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07Metallurgical and Materials Engineering, University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
Figure 4c.4. SSRT Fracture characteristics of LCS strained at a constant rate of 1.6X10-
6/s in air and 100X deaerated YM water at 25 oC and 85 oC. Columns A, B, and C show mechanical test at RT, environmental test at 25 oC, and
environmental test at 85 oC, with imposed Ecorr(-700 mVAg/AgCl). The first row shows half of the fracture surface and the second shows the gauge length
portion at the fracture location.
Metallurgical and Materials Engineering University of Nevada, Reno Results
Mech. test 25oC 85oC
YM-DOE Program Review -DRI, Reno 1-18-07
Inner wall details of QC modes in I-Beam Failed by SSRT at 85oC. The ridges observed with PLC effect, and they showed an average length around 0.4 micron.
Metallurgical and Materials Engineering, University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
B
Metallurgical and Materials Engineering, University of Nevada, Reno Results
SCC tested YM I-beam specimens tested at100x YM water concentration at 85oC.
Scanning electron micrographs of steel sets strained at the rate 10-6/s: (A) Failed in air (B) Using 100x YM water environment.
YM-DOE Program Review -DRI, Reno 1-18-07
Figure 4c.7. Quasi-cleavage(A) and discontinuous planar cleavage(B) crackingmodes of LCS at 85 oC.
Metallurgical and Materials Engineering, University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-0745
50
55
60
65
70
75
80
85
90
500 700 900 1100 1300
Ti ( i t )
Tem
pera
ture
(oC
)
1
23
4
56
-0.74
-0.72
-0.7
-0.68
-0.66
-0.64
-0.62
-0.6
-0.58
550 650 750 850 950 1050
Time(s)
Pote
ntia
l(V);
vs
Ag/
AgC
l
1
2 3
4
56
Metallurgical and Materials Engineering University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
YM-DOE Program Review -DRI, Reno 1-18-07
During strain aging, the interface potential shifts to more cathodvalues. There are precise correlations determined between the amplitudes of serrations and the interface potential, and also corresponding current. This result from this work on I-beam maapply to the other metals as well and the methods can be used investigation tools for understanding PLC effects in depth.
Summary
Electro-mechanical tests methods we used can be useful for investigating PLC Effects in the other metals and alloys.
Metallurgical and Materials Engineering University of Nevada, Reno Results
YM-DOE Program Review -DRI, Reno 1-18-07
Section xx
x x
8”
A B C
YM-DOE Program Review -DRI, Reno 1-18-07
Stress Corrosion Cracking Tests on Yucca Mountain I-Beam Supports Low Carbon Steel (0.08%C) Using SSRT Universal
Testing Machine
-1.2
-1
-0.8
-0.6
-0.4
-0.2
0
1.E-07 1.E-05 1.E-03 1.E-01Log I(A/cm2)
Pote
ntia
l (V)
; vs
Ag/A
gCl
Ecorr
- 620mV- 680mV
AnodicRegion
Cathodic Region
YM-DOE Program Review -DRI, Reno 1-18-07
Actual Swellex Rock bolt-Before Expanding
Idealized Shape before and After Expanding
2B.3
2B.2 (a) 2B.2 (c)
2B.2 (b) 2B.2 (d)
2B.2 (e)
Expanded StateAs Received
YM-DOE Program Review -DRI, Reno 1-18-07
US DOE Sub surface Materials Support Program for the YM Nuclear Materials Storage
DOE Designs
DOE- Approves
Sub surface Metallurgical Materials Evaluation Mainly:
Universities (UNR) –Independent Evaluation of
Various Properties
DOE Site License –Nuclear Regulatory
Commission
Canisters for Nuclear Materials Storage
US National Laboratories –
Lawrence Livermore National Laboratory and
Sandia National Laboratory
Technical Advisory and Scaled testing of Materials
Quality Assurance Program Monitored BY DOE for all our
Potentiodynamic Scans for Rock Bolt at Various Temperatureswith Deaeration by Nitrogen
Anodic
Cathodic
Potentiodynamic Scans for Rock Bolt in Simulated YM Waters(1x)
Effect of Temperature Potentiodynamic Results –Temp.
YM-DOE Program Review -DRI, Reno 1-18-07
-1.2
-1
-0.8
-0.6
-0.4
-0.2
0
1.E-08 1.E-06 1.E-04 1.E-02 1.E+00
Curent Density (A/cm2)
Pote
ntia
l (V)
; vs
Ag/
AgC
l
Polarization of rockbolt in 1X YM water at 25,45,65,85 oC
0
500
1000
1500
2000
2500
3000
3500
4000
0 1000 2000 3000 4000 5000
Re Z(ohms)
Im Z
(ohm
s)
25oC
45oC
65oC
85oC
Impedance Spectra Taken at Ecorr=~-0.75 V
βa. βcB =
2.3 (βa+βc)
Rock Bolt Temperature Effects and Complementary Impedance Spectroscopy on
Medium Carbon Steel (0.44%C) - Deaerated Conditions
Decreasing semi circle radius(polarization resistance) with temperature
Increasing Icorr(Corrosion Rate) with temperature
25oC45oC
65oC
85oC
icorr= B/Rp
Stern-Geary Equation
YM-DOE Program Review -DRI, Reno 1-18-07
-1.2
-1
-0.8
-0.6
-0.4
-0.2
0
1.0E-09 1.0E-07 1.0E-05 1.0E-03 1.0E-01 1.0E+01
Current Density (A/cm2)
Pote
ntia
l(V);v
s A
g/A
gCl
Rock Bolt Concentration Effects of Deaerated Yucca Mountain Waters on at Room Temperature
Polarization of Rockbolts Using 1x,10x and 100x YM waters at 25oC
As expected, there is some Effect of Concentration on Corrosion Behavior of Rock Bolt (RB) in DEAERATED YM waters. CR’s increased slightly with ionic concentration
1x10x
100x
0
500
1000
1500
2000
2500
3000
3500
0 1000 2000 3000 4000Real Z(ohms)
Im Z
(ohm
s)
Impedance Spectra at Ecorr(-0.760 V) for 1x,10x, 100x YM Waters
1x
10x
100x
YM-DOE Program Review -DRI, Reno 1-18-07
020406080
100120140160180
10 20 30 40 50 60 70 80 90 100
Temperature (oC)
Corr
osio
n Ra
te (m
icro
n/ye
ar)
10X
100X1X
Corrosion Rates Showing Temperature and Concentration Effects (Rock Bolts-RB)
Rate (25oC): 30 to 45 μm/yr
Rate (85oC) :160 to 165 μm/yr
Corrosion Rates vs Temp. In the DEAERATED YM Waters With Different Concentrations
Expected small Changes in Corrosion Rates from the 1x to 100x Deaerated YM waters at a given temperature from RT to 85 oC.
25 85
Rate = ___________C. EW. icorr
D
Deaerated
YM-DOE Program Review -DRI, Reno 1-18-07
Polarization plots of I beam samples in Oxygenated 100x solution
-1-0.8-0.6-0.4-0.2
00.2
-8 -6 -4 -2 0
Log (i) A/cm2
Ecor
r(V
) vs
Ag/
AgC
l
25oC (Blue)
45oC (Purple)
85oC (Brown)
65oC (Dark Green)
Temperature Effects on Icorrof I-Beam Using 100x YM
Deaerated/Aerated WatersResults Show CR Peaking at ~45oC Trend for all the YM Concentrations Similar (to RB) in the Next Slide
Polarization plots of I beam samples in Nitrogenated 100x solution
LONG-TERM TES TS (Fille d S ymbols) YMWS = YM Wa t e r S pra y (1x)CH= Cyc lic Humidit y (1x)P I= P a rt ia lly Imme rse d (1x)NI= Non Imme rse d (1x)CI= Comple t e ly Imme rse d (1x)
Nitrogenated
Oxygenated
0
200
400
600
800
1000
1200
1400
1600
0 20 40 60 80 100
Temp erature (C)
μ
273 293 313 333 353 373
Temp erature (K)
1x (Nit rogenat ed))
10x (Nit rogenat ed)
100x (Nit rogenat ed))
1x (Oygenat ed)
10x (Oygenat ed)
100x (Oygenat ed)
YM Wat er Spray
Cyclic Humidit y
K
C H- 12 6 5
Y M W S - 9 70
LONG-TERM TES TS (Fille d S ymbols) YMWS = YM Wa t e r S pra y (1x)CH= Cyc lic Humidit y (1x)
Nitrogenated
Oxygenated
Figure 1(left) Effect of temperature and electrolyte concentration (1,10, and 100x), and oxygen (aerated/deaerated) concentration on the corrosion rate (μm/year) of Rock bolts. Note: the data points in bold symbols with corrosion rates inμm/year are of the conventional (long-term) ASTM Immersion experiments, YM water spray and humidity tests on rock bolt samples.
Figure 1(right) Effect of temperature and electrolyte concentration (1,10, and 100x), and oxygen (aerated/deaerated) concentration on the corrosion rate of I-beam. Note the data points of long-term YM water spray and humidity tests.
Wiliam’s Rock Bolt Low Carbon Steel I–beam from YM site
Summary of Corrosion Rates - 1
YM-DOE Program Review -DRI, Reno 1-18-07
The precipitate layer at 25 °C
Porous scale lets EDX electrons to enter Fe
underneath
Mostly chloride and oxide scales with less
solubility at Low temperatures
The precipitate layer at 85°C
Nonporous and more protective layer
Possible Mg-Si oxide or magnesium chloride
Mn and Fe absence
Scale differences at RT and 85°C on I-Beam Tensile Specimen
Split set-Potentiostatic Scans – Effect of Potential
- 700 mV -600 mV - 400 mV
+200 mV
Fluctuation of current at -700mV and -600mV suggests a formation of unstable pitAt -400mV further increase in current represent a stable pit formation
Results -27
25°C
Swellex Mn24 rock bolt –Potentiodynamic scan-Corrosion Rates Corrosion Rate of Swellex Mn 24 rock bolt in 1X YM water
0
500
1000
1500
2000
2500
25 45 65 90
Temperature(oC)
Cor
rosi
on R
ate
( μm
/yea
r)
De-aerated (Nitrogen)
Aerated (Oxygen)
Corrosion Rate of Swellex Mn 24 rock bolt in YM water concentrations
0
50
100
150
200
250
300
1 10 100
YM water concentration (X times)
Cor
rosi
on R
ate
( μm
/yea
r)
De-aerated (Nitrogen)
Aerated ( Oxygen)
Corrosion rates of Swellex Mn24 rock bolt in aerated conditions are higher at all temperature than in de-aerated conditions.
At ambient conditions, rock bolt corrodes at 30μm/year in de-aerated 1X YM water and 145μm/year in aerated 1X YM water. At 90oC, corrosion rates are 227 and 2269 μm/year for de-aerated and aerated respectively.
In de-aerated and aerated conditions, corrosion rate of rock bolt increased with the concentration. Highest corrosion rate in de-aerated and aerated conditions was observed in 100X solution as 110 and 240 μm/year respectively.
YM-DOE Program Review -DRI, Reno 1-18-07
2.3
2.32
2.34
2.36
2.38
2.4
2.42
2.44
2.46
2.48
0 10 20 30 40 50 60 70 80 90 100 110 120
Time (days)
Mas
s (g
r)
Mass Loss of Rock Bolt in 1x Yucca Mountain Waters at 25oC
Corrosion Rate: 45 micron/year
C
Rate = ____________K x WA x T x D
Experimental set-up
Basic Laboratory Immersion Corrosion Experiment at Room Temperature (25oC)
YM-DOE Program Review -DRI, Reno 1-18-07
Weight Loss of Rockbolt In YM Water at 75 oC.
0.7
0.75
0.8
0.85
0.9
0.95
1
1.05
0 100 200 300 400 500 600
Time(hours)
Mas
s(g)
Effect of Immersion Position at 75oC 1x YM Water
513 μm/yr
960 μm/yr
200 μm/yr
Concentration Cell Effects increases the corrosion rates of rock bolt at the YM water-Humid air borders.• Full Immersion