NSUF Annual Review Increasing... · *Unfortunately there is no single technique that works with all...
Transcript of NSUF Annual Review Increasing... · *Unfortunately there is no single technique that works with all...
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NSUF Annual Review
Increasing instrumentation capability for irradiated nuclear material characterization at Idaho National Laboratory
Fidelma Giulia Di Lemma, Ph.D.Instrument & Metallurgy scientist
PIE & Advanced Characterization DepartmentP.O. Box 1625, MS 6157 Idaho Falls, ID 83415
(208)-533-8005 [email protected]
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from 11/2016,Instrument scientist and metallurgy
2012-2015Ph.D. in applied Sciences
4/2015-10/2016Postdoc on FP and structural material behavior during SA
2006-2011B.Sc.+M.Sc.Nuclear Engineering
1987 Born
2011-2015Intern and grant-holder on aerosol behavior from RDD and SA
Understanding materials
behavior in extreme
conditions
Thermodinamicscalculations
(ThermoCalc, Factsage)
ICP-MS
TG-DTA
Knudsen Cell
X-Ray and Rietveld analyses
+Raman
Spectroscopy
SEM/EDX
+
WDX/EBSD
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NSUF ProjectIncreasing instrumentation
capability for irradiated nuclear material characterization
EPMA (Electron Probe MicroAnalysis) Capabilities
EBSD (Electron BackScatterDiffraction) analyses on reactive
irradiated metals
Metallurgy and instrument scientist
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1) EBSD characterization
EBSD (Electron BackScatter Diffraction) is an analytic technique to evaluate the microstructure of a specimen.
Grain size,
Grain shape,
Grain distribution,
Grain boundary,
Grain orientation,
Deformation and stresses,
Phases determination and inclusions (carbides and precipitates).
The quality of the information dependent upon absolute removal of all surface defects on the sample due to mechanical preparation steps.*
*Unfortunately there is no single technique that works with all materials, and an experimental approach is often required to achieve a suitable result.
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NSUF Task
Goal:
to develop a reliable sample preparation technique for EBSD analyses for reactive metals and especially highly radioactive samples (irradiated/fuel).
Challenges:
Samples are prone to rapid oxidation*, which can influence the EBSD results.
Samples are radioactive and thus must handle following specific safety procedure.
Part 1Analysis of current
techniques and results obtained
Part 2 Proposal of
alternative solution
Part 3Testing of proposed
techniques on various sample
Part 4Develop of a method and
report/publication
*EBSD patterns are generated within a depth of less than 50-100 nm. Because of this, the data quality is extremely sensitive to the integrity of the crystallographic lattice order at the surface of the sample and to oxidation.
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Available techniques in MFCTechnique Pros Contras
1. Mechanical polish (down to 0.05 µm)
Large areas, Available expertise,Multiple samples, Fast (half day ).
Performed in air,Needs a final finishing
2. Vibratory polish Large areas, Available expertise, Multiple samples, alkaline effect
Performed in air, Long (overnight/multiple days).
3. Jet polishLarge areas, Available expertise, Fast
(minutes).Performed in air.
4. EtchLarge areas, Available expertise,
Fast (seconds/minutes)Performed in air, Multiplephases different finishing.
5. FIB/P-FIB(Focused Ion Beam / Plasma Focused Ion Beam)
Good finishing, connected with EBSD, in high vacuum.
Long (hours), small areas.
6. PIPS(Precision Ion Polishing System)
Small areas, Available expertise,Fast (minutes).
Works with small samples.
7. PECS(Precision broad argon Ion Polishing System)
Good results obtained in the past, Available expertise,
Fast (minutes).
Risk of spreading contaminations.
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Possible improvements
Current method Improvements I Improvements 2
1. Mechanical polish 1. Mechanical polish 1. Mechanical polish
2. Vibratory/Jet polish 2. PIPS/PECS 2. Vibratory Polishing
3. FIB/PFIB 3. Transfer tight chamber or specific sample holder or protective layer (coating/spray)
3. Transfer tight chamber or specific sample holder or protective layer (coating/spray)
Current limitations:Long time, Limited FIBs, Oxidation
4. FIB/PFIB on small area of interest
4. FIB/PFIB on small area of interest
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Why PECS?
• Residual oxidation or hydrocarbon contamination is minimal.Lattice damage is on the nanoscale.
• To avoid alteration/contamination* following ion milling, the sample should be transferred to the SEM (Scanning Electron Microscope) immediately.
- Current available machine can be attached directly to SEM chamber.- Current available machine can coat/apply a protective layer directly the sample in PECS.- A transfer chamber could be developed to interface different available instruments.
* Such as dust or dirt on the surface, scratching, formation of oxide layers, moisture.
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Possible plan of action
1. Sample prep with improved
methods
2. EBSD analyses
3. Compare with previous method
Successful?
New sample
YES
Steel
Al/Zr
U*
Irr. steel
Irr. fuel
Sample to test
Method
Implement new techniques
*Collaboration with Dr. D. Murray
NO
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Example benchmarkStainless steel
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2) EPMA• In the EPMA (Electron Probe MicroAnalysis) we bombard a micro-volume
of a sample with a focused electron beam and collect the X-rays emitted.
• WDS (Wavelength Dispersive Spectroscopy) is use to identify the X-rays,and quantify the element present in the sample.
• EPMA is a fully qualitative and quantitative method of non-destructiveelemental analysis of micron-sized volumes at the surface of materials,with sensitivity at the level of ppm.
• EPMA allow simultaneous collection X-ray, SEM, BSE (Back ScatterElectrons) and optical images.
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Advantages
• WDS cannot determineelements below 5 (boron).
• X-rays peaks can overlap andmust be then separated.
• Time consuming.
• Need of accurate standards.
• Need of a complex correctionmatrix.
• Analyses of light elements.
• Quantitative analyses down toppm (High Sensitivity).
• WDS as a better spectralresolution (vs EDS - EnergyDispersive x-ray Spectroscopy).
• WDS better dead time thanEDS.
• Reliable and repeatablemeasurements.
Limitations
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NSUF Task
Goal:
to develop human workforce in operating the EPMA in the INL MFC (Material Fuel Complex) for nuclear and irradiated materials, to support the current instrument scientist.
Part 1Literature
review on the instrument and
analyses
Part 2Training on instrument
Part 3Training on data
analyses
Part 4Perform analyses
independently
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Beam Set up
Instrument conditions and
navigation
Imaging
Peak calibration
Map acquisition
Map Processing
Project Part IIChoice of KV
Filament saturation
Aperture
Beam stability
Instrument Menu operation
Stage movement
Sample and Standard position
Focusing/Astigmatism
Acquisition
Storage
Diffuse vs focused beamCondition for standards
Background selection (from PFE Probe for EPMA)
Acquisition and peak setting
Overlap correction
AutomatizationPeak setting
Beam and optical setting
Mosaic setting
Save method
AutomatizationMosaic Assemblage
Overlap correction
Quantification
Saving
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ExampleIrradiated metallic fuel
SampleFUTURIX-FTA-DOE1
CompositionU-29Pu-4Am-
2Np-30Zr
Irradiation 2.08 x 1021 f/cm3
(9.5% burnup)
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Probe softwareSet up
Standards
Set up
New sample
Set up
ProcessingData
Project Part II TBP
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Conclusion
Increasing instrumentation capability for irradiated nuclear
material characterization
EPMA CapabilitiesEBSD analyses on reactive
irradiated metals
Metallurgy and instrument scientist
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Acknowledgment
This work was supported by the U.S. Department of Energy, Office of Nuclear Energy.
Thanks go to
• Dr. Rory Kennedy for his support and participation in the development of this project
• Dr. Mitch Meyer for his support on these projects.
• Karen Wright, Brandon Herrandez, Tammy Townbridge, Jason Harp for their technical advice, support in data collection and elaboration.
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Reference• E.A. Fischione Instruments, Application Note “Metallic sample preparation for EBSD by
mechanical method and argon ion beam milling” AN012 Revision 01 04/2014
• Streurs, Application Notes “Preparation of ferrous metals for Electron Backscatter Diffraction (EBSD) analysis” 02.2010 / 62140410
• M.M. Nowell, R.A. Witt, and B.W. True “EBSD Sample Preparation: Techniques, Tips, and Tricks”, Microscopy today, p. 44-48 July 2005
• Oxford Instrument Application note “EBSD Sample preparation”
• S. Suwas, and R.K. Ray “Crystallography Texture of Materials” 2014, XIII, p. 260.
• Thermoscientific “Wavelength dispersive (X-ray) Spectroscopy” Essential Knowledge Brifieng, 2016.
• CAMECA_SXFiveFE_2_page_flyer.pdf
• https://www.bruker.com/fileadmin/user_upload/8-PDF-Docs/X-rayDiffraction_ElementalAnalysis/XRF/Webinars/Bruker_AXS_EDX_vs_WDX_Webinar_Slides.pdf
• https://www.ems.psu.edu/~ryba/harbin/EPMA.ppt.pdf
• http://etd.library.vanderbilt.edu/available/etd-07192013-160603/unrestricted/Hammonds.pdf
• http://tech.snmjournals.org/content/32/3/139/F4.expansion.html
• https://www.jeolusa.com/RESOURCES/Electron-Optics/Documents-Downloads?EntryId=5
• http://www.ebsd.com/
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WDX
Detector RangeK line
RangeL line
RangeM line
TAP F(9)-P(15) Mn(25)-Y(39) La(57)-Ir(77)
PET Si(14)-Cr(24) Sr(38)-Eu(63) W(74)-Pu(94)
LiF Sc(21)-Br(35) Te(52) to Bi(83) N.A.