Transcript Post Irradiation Examination of an Alloy 718 Beam Window Stuart A. Maloy1, Hong Bach2, Tarik A.

Post Irradiation Examination of an Alloy
718 Beam Window
Stuart A. Maloy1,
Hong Bach2, Tarik A. Saleh1, Tobias J. Romero2,
Osman Anderoglu1, Bulent H. Sencer3
1. Materials Science and Technology Division -Los Alamos National
Laboratory
2. Chemistry Division -Los Alamos National Laboratory
3. Idaho National Laboratory
(May 21, 2014)
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Outline
 Isotope Production Facility
 Cutting of Window and Dimensional Measurements
 Calculation of Dose and Irradiation Temperature
 Shear Punch Testing
– Trepanning of Specimens
– Dose/Irradiation Temperature vs. Location
– Shear Punch Testing and Data
 TEM Analysis
 Comparison to previous test results
 Summary
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Isotope Production Facility LANSCE
H+ is produced at the source
injector, accelerated through DTL,
diverted to IPF at the TR region
through magnets, and ended on
targets inside a heavily shielded
target irradiation chamber .
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Isotope Production Facility and Beam
Window
Steel
Proton
Beam
Beam window
Target carrier
The proton beam is delivered via a vacuum beam pipe. Inconel 718 beam
window isolates the beam pipe (under vacuum) and the target irradiation
chamber (15 psig of cooling water).
Present design limit for window is 5 years and would like to increase that
limit through analyzing properties after 5 years of operation.
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Cutting off the Window
Window was cut from beam
tube remotely in the corridor
of the CMR Wing 9 hot cells
Then, the window was
placed into an individual hot
cell for analysis and sample
preparation.
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Dimensional and Dose Measurements
on Window
100
10
5
120
4
6
9
11
8
140
7
B (gray)
160
12
3
180
200
220
2
240
-5
0.040
0
13
5
measurement (in.)
10 15 20 25 30 35 40 45 50 55 60 65 70 75 80
mm
0.030
0.020
contour (TB)
0.010
0.000
contour (LR)
-0.010
-0.020
thickness
(T-B)
-0.030
-0.040
thickness
(L-R)
-0.050
-0.060
GAFCHROMIC HD-810
dosimetry film was used to
measure the absorbed dose
of high energy photons from
the activated beam window.
↓vaccum side ↓
-0.070
-0.080
0
0.5
1
1.5
2
2.5
3
distance (in.)
Beam window deformed 1.5mm
into the vacuum side.
Rastered beam profile shows a Gaussian
distribution and the highest dose region
corresponds to the darkest blue region on the
Gafchromic film.
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Temperature and Dose Map
0.25-1.5 dpa
109C
2-5 dpa
12.5 dpa
9.5 dpa
25C
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Cutting and Shear Punch Testing
Plan




Samples Tested
Samples Cut but Untested
Black Circles were not cut
Beam profile was superimposed on the
window to determine the cutting plan
as a function of radiation dose (dpa).
3-mm OD samples were cut with a Mill
machine. A total of 3 cutting bits were
spent to cut out 20 numerical samples
(1-20) and 5 alphabetical samples (A, B,
C, E, and F).
Cut-out samples were polished and
thinned from on both sides to 0.254 mm
thickness.
The shear punch testing for the
following samples were completed as a
function of radiation dose (dpa):
•
•
2 controls samples of unirradiated
Inconel 718
1-6, 8, 9, 10-13, 15-16, 17-18, 19-20, A-C,
and E
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Trepanning 3 mm Diameter
Samples from Window
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Shear Punch Testing Equipment at
CMR Hot Cell
Loading
Direction
0.600 "
3mm
diameter
disk
Disk Sits Here
1 mm Punch
0.25mm
thick
1mm
diameter
punch
Sample Disk


Shear Punch Set-up

Performed 25 shear punch tests on
3 mm diameter specimens.
Tested at initial strain rate of 5 x 104/s.
Tested at in ultra high purity argon.
Loading sequence
Typical shear punch specimen
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Control Material Tensile Tests vs Shear
Punch
UTS
correlation -
1.28
Yield
Correlation-
1.77
Lit
values 1.4, 1.73
Toloczko&Kurtz
3 controls in-cell process
700 MPa UTS
800
Effective Shear Strength (MPa)
700
600
500
400
Control 4
300
230-250 MPa
1%shear yield
200
Control 5
100
Control6
0
0
0.05
0.1
0.15
0.2
Displacement (mm)
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0.25
0.3
Shear Punch, Outer to Inner
Control + 4 regions
1000
Effective Shear Stress (MPa)
0.5dpa
2.55dpa
11 dpa
800
12.5 dpa
600
Control
400
High Rad 3
High Rad 4
Outer Ring 17
Outer Ring 18
Beam Center 1
Beam Center 2
Outside Collimator 10
Outside Collimator 11
Control
200
0
0
0.05
0.1
0.15
0.2
0.25
0.3
Displacement (mm)
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Comparison of Shear
Stress/displacement Curves
OuterRing
1000
HighRad Ring
Effective Shear Stress (MPa)
800
Effective Shear Strength (MPa)
700
600
500
#3
400
#4
#5
300
#6
200
800
600
#17
#18
400
19
20
200
#8
#9
100
0
0
0
0.05
0.1
0.15
0.2
0.25
0
0.05
0.1
0.15
Displacement (mm)
Displacement (mm)
Dose = 12.5 dpa
Dose = 0.5 dpa
Tirr= 109C
Tirr=50C
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0.2
Optical Images of Exit side of
Shear Punch Specimens
Control Material
Dose = 12.5 dpa
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Inconel 718 Solution Annealedunirradiated
Bright field TEM images showing dislocations and some
precipitates
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TEM Analysis of Irradiated Alloy 718 Samples
z=[111]
0.5 dpa at 50°C
z=[001]
z=[001]
12.5 dpa at 109°C
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Previous Results on Proton
Irradiated Annealed 718 SPF
STIP-II Inc 718 SPF Shear Punch Tests
STIP-II Inc718 SPF Tensile Tests
1000
1400
7.0 dpa, Tirr=147 C,
~500 appm He
7.8 dpa, Tirr=183C,
~600 appm He
900
18.7 dpa, Tirr=406 C,
~1700 appm He
1200
18.4 dpa, Tirr=382C,
~1700 appm He
800
Control
Effective Shear Strength (MPa)
Stress (MPa)
1000
800
600
400
700
Control
600
500
400
300
200
200
100
0
0
0
5
10
15
20
25
30
35
40
45
50
55
Strain (%)
0
0.05
0.1
0.15
0.2
0.25
0.3
Displacement (mm)

Inconel 718 SPF samples irradiated in STIP-II

Samples show good retention of ductility even with much higher helium levels
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Summary of Tensile Results
Tensile Yield vs. Position
109C
1200
0.25-1.5 dpa
2-5 dpa
9.5 dpa
25C
Tensile Yield Stress (MPa)
12 dpa
1000
2-4 dpa
@40C
9-10 dpa
800 @ 40C
0.2-0.9 dpa
@ 50C
11.7 dpa 12.5 dpa
@109C
@75C
600
Control
400
200
0
0
0.2
0.4
0.6
0.8
1
Radial Position (in.)

All samples display ductility in both yield vs UTS and optically.

Samples taken in outer ring and outside collimator have a higher yield and UTS
than control or high radiation dose samples.

Increased hardening appears to be a combination of increased defect density,
bubble density and second phase precipitation

From these results we are confident to push lifetime out to ~17 dpa

Further analysis required
toAlamos
understand
formation
in low
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1.2
1.4
Comparison to previous tensile results
 Farrell et al. (03) shows increase from 350 MPa
to 900 MPa for irradiation at 50-100C for a dose
of 1.2 dpa
 STIP-II shows increase from 600 to 1200 MPa at
183C and 600 to 1100 MPa at 382C to doses of
7.8 and 18 dpa respectively
 IPF data shows increase from 450 to 1100 MPa
at 9 dpa and 850 MPa at 11-12 dpa. Also an
increase to 1100 MPa is observed at 2-4 dpa.
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Shear Punch Results
Almost All Middle Range
Around the Outside of Colimator
HighRad Ring
1000
800
1000
700
#1
#2
#3
#4
#5
#6
500
#3
400
#4
#5
300
#6
200
#8
200
Effective Shear Stress (MPa)
Effective Shear Strength (MPa)
600
400
600
#8
800
600
10
11
12
400
13
15
16
200
#9
#9
100
#A
0
0
0
0.05
0.1
0.15
0.2
0
0.25
0.05
0.1
0.15
0.2
0
0.25
0.05
0.1
0.15
0.2
Displacement (mm)
Displacement (mm)
Displacement (mm)
OuterRing
Control + 4 regions
1000
1000
800
Effective Shear Stress (MPa)
0
Effective Shear Stress (MPa)
Effective Shear Strength (MPa)
800
600
#17
#18
400
19
800
600
400
High Rad 3
High Rad 4
Outer Ring 17
Outer Ring 18
Beam Center 1
Beam Center 2
Outside Collimator 10
Outside Collimator 11
Control
200
20
200
0
0
0.05
0.1
0.15
0.2
0.25
Displacement (mm)
0
0
0.05
0.1
0.15
0.2
Displacement (mm)
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0.3
0.25
Dark and bright field TEM images showing
smaller precipitates and dislocations.
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Unirradiated Inconel 718
Co, Cu) rich precipitate
Ni, Mo, Nb (some
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Inconel 718 #5 ~14 dpa @109°C
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Irradiation Damage and Replacement
 Beam transmission through the window incurs heating causing thermal stress.
 Beam irradiates the window causing mechanical properties to change.
 Beam window design criteria is 20 dpa (displacement per atom). Beam window
reached the end of its life.
 Estimate dose rate is 100 R/hr at contact without shielding and highly contaminated.
 We replaced window in March 2010, stored at Area A and shipped to CMR in
November 2010.
Calculated Von Mises stress under
pressure and thermal load at the
center of the target is ~ 510 MPa.
Window will fail when Von Mises
stress > the yield strength
718 Yield
Dose, dpa
15
20
18
End of run cycle 2009
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Image of Beam Window Surface
Outline of beam
collimator is evident
on beam window
Approximate
dimensions are 10 cm
diameter x 0.5 mm
thick.
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Machined Window
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Optical Images of Control Sample #6
(Unirradiated)
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Optical Images of Sample # 8 (High
Radiation Ring)
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z=[111]
Reference: M. Dehmas et al. Advances in Mat. Sci. and Eng (2011)
Unirradiated (SA)
z=[001]
z=[001]
0.5 dpa at 50°C
z=[001]
12.5 dpa at 109°C
z=[001]
°C
Unirradiated-PHOperated by Los Alamos0.5
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Inconel 718 #19 ~ 0.5 dpa @50°C
under focus
under focus
109C
0.25-1.5 dpa
Bright
field TEM images showing
dislocation loops.
Under-focus
TEM images on the right are
showing a high
Density
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arebyon
25C
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Inconel 718 #19 ~ 0.5 dpa @50°C
g“ precipitates
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0.5 dpa 50°C
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Inconel 718 #16~ 2.5 dpa @ ~40°C
109C
2-5 dpa
25C
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Inconel 718 #5 ~12 dpa @109°C
109C
12dpa
Bright field TEM images
showing dislocations,
precipitates are not detected?
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25C
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Inconel 718 #E ~11 dpa @~75°C
109C
11 dpa
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25C
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Loop size and density
Reference: M. Dehmas et al. Advances in Mat. Sci. and Eng (2011)
size
Loop density
Loop
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