materials characterization of tantalum for high energy ... · this work performed under the...
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Lawrence Livermore National Laboratory
Kerri Blobaum Bassem El-Dasher, Mukul Kumar, Jeff Florando, Rick Gross, & Dave Swift
LLNL-PRES-501632
Lawrence Livermore National Laboratory, P. O. Box 808, Livermore, CA 94551 This work performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344
Materials Characterization of Tantalum for High Energy Density Targets
May 24, 2012
2 Lawrence Livermore National Laboratory
The morphology, processing, and preparation of a target material can be as important as its chemical composition
MECHANICAL PROPERTIES Strength Ductility
MORPHOLOGY Grain size
Grain shape Texture
FABRICATION Polishing Cutting
Deformation
CHEMICAL COMPOSITION Impurity levels
Location of impurities Impurity composition
PROCESSING Rolling
Annealing Sputtering
3 Lawrence Livermore National Laboratory
OMEGA and NIF experiments are designed to study mechanical properties of materials at high pressures and high strain rates
Rayleigh-Taylor experiments for validation of strength models
• RT instability develops when a less dense fluid pushes a more dense fluid
• Strength of the material slows growth • Instability growth measured with VISAR
Hydrodynamics simulation of RT growth
Shengtai Li & Hui Li, “Parallel AMR Code for Compressible MHD or HD Equations,” LANL Report LA-UR-03-8926 http://www.physicscentral.com/explore/pictures/cup.cfm
High density liquid on top of a lower density liquid
4 Lawrence Livermore National Laboratory
Rayleigh-Taylor instabilities are seeded with sine-wave ripples on tantlum in OMEGA and NIF targets
Ripple Dimensions • Peak-to-valley amplitude: 1 – 7 µm • Wavelength: ~50 µm
Compression screw
Spring
Load cell
Plunger
Die (flat)
Punch (contoured)
Displacement gauge
Press for coining sine-wave pattern
500 µm
500 µm
5 Lawrence Livermore National Laboratory
A 5 Mbar drive for Ta Rayleigh-Taylor experiments was demonstrated at NIF in March 2011
Fully assembled target with VISAR and unconverted light shields
View of the target package, looking down the VISAR shield
Assembly drawing
Side view of the target package (LiF & quartz windows, Ta foil, Al spacer, foam
reservoir encased in epoxy)
Face-on view of the target package mounted on the outside of a hohlraum
5 mm
5 mm 2 mm
1 mm
6 Lawrence Livermore National Laboratory
RT experiments measure material properties; it is important to select, process, and characterize tantalum carefully
Not all high-purity tantalum is the same!
Microstructure of rolled Ta (pancaked grains)
Equiaxed grains
Rolling produces non-equiaxed grains
Most commercially available foils are rolled
Rolled and annealed
400 µm
100 µm
100 µm
7 Lawrence Livermore National Laboratory
In a “textured” material, the grains have a preferred crystallographic orientation
From J.F. Schackelford, Introduction to Materials Science for Engineers, 1988.
Random orientation Textured
8 Lawrence Livermore National Laboratory
We use electron backscatter diffraction (EBSD) to measure texture and grain size
11.559
3.268
<0.924
MRD
Orientation map
Grain size distribution
Pole figures
Grain size (µm) 10 100
9 Lawrence Livermore National Laboratory
A piece of material can have a preferred orientation in one direction, while randomly oriented in others
ND
RD
TD
ND
RD
TD
The top face of the block has a preferred 111 orientation
The sides of the block have a preferred 101 orientation
ND
TD RD
Pole figure for normal direction
ND = normal direction TD = transverse direction RD = rolling direction (note: this is not necessarily the direction in which the sample was rolled
10 Lawrence Livermore National Laboratory
Tantalum is notoriously inhomogeneous with respect to grain size and texture
Banding readily occurs, even over small length scales
1 mm 1 mm
11 Lawrence Livermore National Laboratory
Characterization of tantalum is essential, given its propensity for inhomogeneity
500 µm
500 µm
12 Lawrence Livermore National Laboratory
The morphology, processing, and preparation of a target material can be as important as its chemical composition
MECHANICAL PROPERTIES Strength Ductility
MORPHOLOGY Grain size
Grain shape Texture
FABRICATION Polishing Cutting
Deformation
CHEMICAL COMPOSITION Impurity levels
Location of impurities Impurity composition
PROCESSING Rolling
Annealing Sputtering
13 Lawrence Livermore National Laboratory
Grain size affects material strength (Hall-Petch relation)
Strength is inversely related to grain size (Hall-Petch equation)
Grain size is typically measured with optical or scanning electron microscopy
σy = yield stress
σ0 = frictional stress required to move dislocations
ky = “locking parameter” (relative hardening contribution of grain boundaries)
D = grain size
From M.A. Meyers & K.K. Chawla, Mechanical Metallurgy, 1984.
14 Lawrence Livermore National Laboratory
The strength of tantalum is also a strong function of orientation (texture)
J.F. Byron, Journal of the Less-Common Metals, 1968.
Yield strength of oriented single crystals
Strain rate = 4 x 10-4/s
Tension
Compression
[001]
Yiel
d st
ress
(kg/
mm
2 )
[011]
[111]
[001]
[001]
Yiel
d st
ress
(kg/
mm
2 )
[011]
[111]
[001]
15 Lawrence Livermore National Laboratory
The morphology, processing, and preparation of a target material can be as important as its chemical composition
MECHANICAL PROPERTIES Strength Ductility
MORPHOLOGY Grain size
Grain shape Texture
FABRICATION Polishing Cutting
Deformation
CHEMICAL COMPOSITION Impurity levels
Location of impurities Impurity composition
PROCESSING Rolling
Annealing Sputtering
16 Lawrence Livermore National Laboratory
Small amounts of impurities can dramatically affect the strength of tantalum
T.E. Tietz and J.W. Wilson, Behavior and Properties of Refractory Metals, 1965.
Har
dnes
s (D
HN
)
Interstitial content (at. %)
Interstitial impurities Oxygen content
Oxygen content (wt. %)
Air
Nitrogen
Oxygen
17 Lawrence Livermore National Laboratory
The morphology, processing, and preparation of a target material can be as important as its chemical composition
MECHANICAL PROPERTIES Strength Ductility
MORPHOLOGY Grain size
Grain shape Texture
FABRICATION Polishing Cutting
Deformation
CHEMICAL COMPOSITION Impurity levels
Location of impurities Impurity composition
PROCESSING Rolling
Annealing Sputtering
18 Lawrence Livermore National Laboratory
Sputter-deposited Ta has a highly defected, columnar morphology, which affects mechanical properties
Plan view Cross-section
100 nm 200 nm
19 Lawrence Livermore National Laboratory
Compared to a commercially available Ta foil, sputter-deposited Ta is significantly harder
Vickers Hardness = 137.7 Vickers Hardness = 208 Commercially available foil Sputter-deposited foil
Plan view
Cross-section
200 µm
200 µm
1 µm
2 µm
20 Lawrence Livermore National Laboratory
The morphology, processing, and preparation of a target material can be as important as its chemical composition
MECHANICAL PROPERTIES Strength Ductility
MORPHOLOGY Grain size
Grain shape Texture
FABRICATION Polishing Cutting
Deformation
CHEMICAL COMPOSITION Impurity levels
Location of impurities Impurity composition
PROCESSING Rolling
Annealing Sputtering
21 Lawrence Livermore National Laboratory
Artifacts can be introduced during target fabrication
Cutting/thinning operations • Polishing can leave surface damage • Electro-discharge machining can introduce
impurities Coining
• Results in increased hardness
22 Lawrence Livermore National Laboratory
Aggressive polishing can leave a layer of deformed material on the surface of the target
Polishing damage
Polishing damage
23 Lawrence Livermore National Laboratory
The surface layer damaged by polishing is harder than the underlying material
Hardness values obtained from nanoindentation
1.77 GPa
1.5 GPa
2.09 GPa
1.48 GPa
24 Lawrence Livermore National Laboratory
In tantalum, we discovered that polishing to approximately 50 µm thick results in deformation banding
Plan view SEM Cross-sectional SEM
Plan view SEM
50 µm
10 µm
10 µm
25 Lawrence Livermore National Laboratory
Deformation bands in thin tantalum foils are small angle misorientations—not twins
Backscatter SEM micrograph of area scanned at high resolution
EBSD Scan Area
[001]S Inverse Pole Figure Map of scan area
26 Lawrence Livermore National Laboratory
Deformation bands in thin tantalum foils are small angle misorientations—not twins
5 °
2.5 °
0 °
Deviation
Twins would have a misorientation angle of 60°
Mis
orie
ntat
ion
(deg
rees
)
1.2
0.5
0.0 0 5 1.2
Distance (µm)
Point-to-point Point-to-origin
27 Lawrence Livermore National Laboratory
Annealing appears to remove most of the deformation banding
Pre-annealing Annealed at 980°C for 30 minutes (UHV)
Debris is due to laser cutting and previous mounting medium
10 µm
10 µm
25 µm
25 µm
28 Lawrence Livermore National Laboratory
The morphology, processing, and preparation of a target material can be as important as its chemical composition
MECHANICAL PROPERTIES Strength Ductility
MORPHOLOGY Grain size
Grain shape Texture
FABRICATION Polishing Cutting
Deformation
CHEMICAL COMPOSITION Impurity levels
Location of impurities Impurity composition
PROCESSING Rolling
Annealing Sputtering