Post on 15-Jul-2020
Office of Researchand DevelopmentNanoscale,X.ray,Computed,Tomography,of,Solid,Oxide,Fuel,Cell,Electrodes
William,K,EptingU1.3,Shawn,LitsterU3,Kirk,GerdesU1,Paul,A,Salvador1U2,,,
,,,,1National,Energy,Technology,LaboratoryU,UDSD,Department,of,Energy;,2Dept,of,Materials,Science,and,EngineeringU,Carnegie,Mellon,UnivD;,3Dept,of,Mechanical,EngineeringU,Carnegie,Mellon,UnivD
Acknowledgment:"s- part- of- the- National- ±nergy-Technology- µaboratory5s- research-portfolioC- this- work- was- conducted-under-the-R±S-contract-?±v%±222*222
UsingbabSphericalbDilatingbKernelbofbRb=bW:
Niµarge-pores
NivYSZC-pores
YSZC-no-pores
µSMvYSZC-pores
µSMµarge-pores
(2-μm
V2-μm
V2-μm
82-μm
~(22-μm
Hathodecurrentcollector
"ctive-cath.
"ctive-anode
±lectrolyte
"nodesupport
R-P-8
Hoarser-kernels
R-P-x
Spherical-kernel N8:-kernel Hubic-kernel
Startingvoxel
Dilate
YSZ
µSM
Void
YSZ1
µSM
Void
YSZ1
µSM1
Void1
YSZ1
µSM
Void1
Void
µSM
YSZ
Void
YSZ
YSZ-mbright3
Ielowresolution
limit
Iorderregion
Raw-virtual-x?-slice
IutC-thereal
structurelooks like
this•
Void-mdark3
Void µSM YSZ
Segmentation
greyscales-based-on-real-volumes-of-µSM-
elsewhere
RemovalbMethod:bMorphologicalbDilationThreexPhasebArtifact
Artifactbremovalbbybsequentialbdilationb
µSM-artifact-coating-all-YSZ-mthere-should-be-YSZvpore-interfaces3
µSM-artifact-even-coating-electrolyte-layer-mnot-physical3
Dilation:bDifferentbkernelsbandbsizes
StudyingbDilationbParametersbforbArtifactbRemovalReasonable-outcomes Unreasonable-outcomesUntreated
Isbit
phys
ical
?Ef
fect
bon
phas
ebfr
ac?
Effe
ctbo
npo
rebc
onta
ct?
Effe
ctbo
nph
aseb
perc
olat
ion?
Kernel: cubeRadius: 3
• AllRfeaturesRlookRvery“cube<ified”
• LSMRreducedRtoRsingleisolatedRcubes
VirtualR/DRslice
ThinnestRLSMRskinsgone
RemainingRLSMRthickenoughRtoRbeRreal
Qualitatively, shapesfaithful to orig. data
LSMRcovering all
YSZ < notRphysical
VoidYSZLSM
VirtualR/DRslice
LongRlimbspresent%Rsmallerthan nano<CT’sresolutionRlimit
Kernel: faces onlyRadius: 2
LSM
YSZ VoidElectrolyte
region
Z coord.-[μm]
Pha
se-f
ract
ion
LSMRFractionR>RPw,Not likely true.
LSMRlikelyRgettingboostRinRvolumeRfrom
artifact
LSM
YSZ VoidElectrolyte
region
Pha
se-f
ract
ion
LSMR<3z,RseemsunreasonablyRlow
Cube%RradiusRx
LSM
YSZ VoidElectrolyte
region
Sphere%RradiusR/
Z coord.-[μm]
zw,RLSMRseemsRhigh%RbutRpossiblemHommercial-composition-unknown3
LSMYSZ
VoidElectrolyte
region
Sphere%RradiusRx
Z coord.-[μm]
xw5xw5xw,RmixRalsoRseemsreasonable
LSM
YSZElectrolyte
region
Por
e-ex
posu
re
LSM<poreRexposurehasRtakenRaRlargeRhit
Cube%RradiusRx
LSMYSZ
Electrolyte
region
Sphere%RradiusR/
Z coord.-[μm]
YSZ<poreRexposureRhasRcomeRfromR~wtoRaRmeasurableRamount%RLSM<pore
exposureRstillRsizeableLSM
YSZ
Electrolyte
region
Sphere%RradiusRx
Z coord.-[μm]
YSZ<poreRandRLSM<poreRveryevenRnow%RthoughRTPBRmaybeRaboutRtheRsameRasRabove
LSM
YSZ
Electrolyte
region
Z coord.-[μm]
Por
e-ex
posu
re
YSZRhasRvirtuallyRwRcontactRwithRpores1
Unprocessed Sphere%RR=/ Sphere%RR=x Cube% R=x
Kernel:HsphereRadius:H2
YSZ-connectivity-pretty-reasonable-to-begin-with.
Void-connectivity-lowC-but-some-dead-pores-expected.
Void-connectivity--higher-v-closer-to-expected-characteristics.
"ll-three-phases-have-excellent-connectivity.
µSM-connectivity-has-been-severely-diminished-by-overvdilation.
Radiograph
±lectrolyte
V2-μm
V?-reconstruction
Virtual-x?-slices
Raw Segmented
NanoscalebXxraybCTbofSolidbOxidebFuelbCells
Hathode-materials•µSM
YSZ
µanthanum-strontiummanganateC-electronconductor-=-catalyst
YttriavstabilizedzirconiaC-oxide-conductor
%OV
X-rayHCTHwithH65HnmHresolution
LDbSpatialbAnalysisbofbTPBbDistribution
Shaftvlike-0dead-zone0
HeterogeneitybAnalysis
OngoingbWork:bAdvancedbSamplebPrepbforbLargerObMorebRepresentativebSamples
m*-μm3V
TPIs-determined-vertexvbyvvertex-in-V?
Vetices-connected-to-orthogonal-neighbors
Paths-smoothed-for-accurate-length-measurement
µocal-TPI-length-stored-on-voxelvbyvvoxel-basis-for-V?-spatial-analysis
82x82x(-μm-region-selected-for-heterogeneity-analysis-mbelow3
TPB density "cloud" visualization
Multiple-cubic-ROqs-placed-within-larger-volume
+ow-much-does-TIP-density-differ-between-each-cubeC-as-the-cubes-become-smallerz
Typ-.-%qIvS±M-size
±*2Zdeviation- from- mean-TPIC- based- on- U(Z-confidence- interval-on-Tvdistribution
µarger- volumes- mV2~- μm3- required- to-accurately-characterize-more-heterogeneous-industrial-cells-v-nanovHT-is-capable
N-P
-V)
N-P
-8*
N-P
-*
qdeal-sample0%racture- and- hope0- method-may- favor- statistically- unusual-samples•- 0why- did- it- break-therez0
qn- factC- this- sample- is- more-homogeneous-than-many-other-samples- previously- attempted-in- %qIvS±MC- which- exhibited-large- superporesC- or- *~- μm-boulders-of-solid-material.
Cut-and-polishHmethod
?irection-of-polishing
Hut Polish
Micrometervcontrolled-
fixture
Trim-with-laser ±xtract-pillar
Mount-vertically-for-nanovHT
AbstractUnderstanding- performance- degradation- in-SO%Hs- requires- an- understanding- of-electrode-microsctructurePrior-methods-yield-small-fields-of-view-below-scale-of-eterogeneity-present-in-some-cellsNanoscale- Xvray- HT- can- yield- V?- - -microstructure-of-a-larger-volume
Here,HweHpresentHimaging,HartifactHremoval,HandHanalysisHofHtheHscaleHofHheterogeneityHinHHindustrialHSOFCHelectrodes
Virtual-x?-slice-from-V?-image
82-μm
µSM
YSZPore ±
lect
roly
te
2.x 2.* 2.) 2.:2
(
82
8(
x2
x(
YSZµSM Pore
Z-c
oord
-[µm
]
Vol-fraction
Phase-fraction-analysis
Hur
rent
-col
lect
or
Phase-connectivity-analysis
AnalysisHofHlargerHcathodeHvolumeH445HxH32HxH25Hμmx
µSM YSZ Void2
2.x
2.*
2.)
2.:
8
µarg
est-c
ontig
uous
-frac
.
z