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Characterization of Particles d V id U i X Miand Voids Using X-ray Micro

TomographyTomographyBrian M. Patterson, E.K. Cerreta, D. Dennis-Koller, C.A.

B kh t d C E H iltBronkhorst, and C. E. Hamilton

Los Alamos National Laboratory, Los Alamos, NM 87545

Tomography Workshop 2010

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OverviewOverview

How many radiographs do you need for y g p ydimensional quantification?

How many voxels do you need for object How many voxels do you need for object particle statistics, not image artifacts?

Dynamically damaged Cu Dynamically damaged Cu

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Xradia Micro Computed TomographyXradia Micro Computed Tomography

150 kV, 10W, W-source2 glass slides for beam hardening10X objective ~2.5 mm FOV2.24 μm voxel size

17~24 hrs per sample for best image quality

Great for meso scale features

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Analysis Using AvizoFireAnalysis Using AvizoFire3D image analysis using AvizoFire 6.2g y g

64-bit, HP workstation, Windows 7, Nvidia FX-5600 graphics card with 4gb ram

The use of μCT lends 3D statistics to traditional 2D characterization. Exciting new capability and g p yextremely useful if implemented carefully.

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Calibrated Volume MeasurementsCalibrated Volume MeasurementsEmbedded solid NIST standard beads in 60 mg/cm3 polymer

3D image of NIST standard beads using X-ray CTvaried the number of x-ray images to determine

1. can beads be used as standards2. are the 3D measurements accurate

Data sets of:181, 361, 721, 1261 images collected

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PATTERSON, B.M. & HAMILTON, C.E. (2010). Analytical Chemistry 39(3), 184-190.

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Photomicrograph of glass spheresg p g p

Geometry of x-ray tomography instrument

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PATTERSON, B.M. & HAMILTON, C.E. (2010). Analytical Chemistry 39(3), 184-190.

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Reconstructed slices through sphere embedded polymer

1261 721

Reconstructed slices through sphere embedded polymer

361 181

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PATTERSON, B.M. & HAMILTON, C.E. (2010). Analytical Chemistry 39(3), 184-190.

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Histogram of binary particlesHistogram of binary particles

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PATTERSON, B.M. & HAMILTON, C.E. (2010). Analytical Chemistry 39(3), 184-190.

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20 micron beads, 1261 images, g

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PATTERSON, B.M. & HAMILTON, C.E. (2010). Analytical Chemistry 39(3), 184-190.

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Average bead diameter calculation comparison

1261

Average bead diameter calculation comparison

NIST Standard 1261 Radiographs 721 Radiographs 361 Radiographs 181 Radiographs

Average Bead Diameter

(μm) and SD17.3 ± 1.4 18.4 ± 1.9 17.8 ± 1.9 17.4 ± 1.9 17.0 ± 1.9

(μm) and SD

R l ti %Relative % SD 12 10.7 10.8 11.1 11.2

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PATTERSON, B.M. & HAMILTON, C.E. (2010). Analytical Chemistry 39(3), 184-190.

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How many voxels?How many voxels?

No one would believe that the surface area of a single voxel object is accurate!What about a 5 voxel object? jWhat about a 50 voxel object?

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27 cylinders in various resampled datasets

9003 1003 253

27 cylinders in various resampled datasets

900 100 25

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Slice through one cylinder in various resampled datasets

9003 1003 253

g y p

9003 1003 253

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Define Feret Shape 3DDefine Feret Shape 3D

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Accuracy measures as a function of the ynumber of object voxels

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Precision measure of the cylinders as f i f b f la function of number of voxels

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Numerous industrial applications call for damage tolerant materials in extreme environments

Crash WorthinessVulnerability and Safety

Structural Integrity

Foreign Object Damage

A future of materials with designer properties relies on our capabilityU N C L A S S I F I E D

A future of materials with designer properties relies on our capability to understand and predict the response of such materials in the

extreme environments of stress, strain, temperature, and pressure.

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Experimentally we mimic this effect through gas gun, laser drive or high explosive loading platformsg p g p

Damage in a shocked specimenquartz Cu targetm

e

impactor targetup

t tim

x

Flat top loading

(supported)

t

Discreet

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Discreetregion of tension

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3 2 1About ~ 7 mm available for analysis

h= ~ 4 2 mmHigh purity OFHC copper

h= ~ 4.2 mm

thickness = ~ 1.7 mmthickness 1.7 mm

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Shocked SamplesShocked Samples

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Flow chart for segmentation

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Smoothed Arithmetic

Dilation MaskDilation Mask

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Smoothed 3D image of voids in damaged Cug g

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Feret Shape Cut-Offp

All voids with 1000 voxels or moreAll voids

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Is it accurate?Is it accurate?

Void volume by 2D areay0.41%

Void Mass Void Mass0.42%

CT CT0.64%

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Cu damaged at higher velocityCu damaged at higher velocity

3 t3mm quartz171 m/s

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Normalized Radius of Voids40

30

20

mbe

r of V

oids

10

Num

113 total number of voids with a volume greater than 27 voxels

0 50 100 150 2000

g

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Normalized Radius (micrometers)

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Binary and Labeled Reconstructed Slicey

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Normalized Radius of Voids

35

40

Individual voids

Normalized Radius of Voids

30

35 Individual voids

20

25

ber o

f Voi

ds

10

15

Num

b

Large void virtually separated

0 50 100 150 2000

5 Congealed void

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0 50 00 50 00

Normalized Radius (m icrometers)

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SummarySummaryX-ray Micro CT coupled with high end image processing provides a non-destructive 3D characterization of meso scale damage structures in a laboratory based environment. Information on the resultant process’ are imaged; not available in typical 2D cross sectioning.

Now we can balance resolution versus field of view.

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AcknowledgmentsAcknowledgments

Funding was provided by the LaboratoryFunding was provided by the Laboratory Directed Research and Development program(LDRD DR 20100026)(LDRD-DR-20100026)

PATTERSON B M & HAMILTON C E (2010) Analytical Chemistry 39(3) 184 190PATTERSON, B.M. & HAMILTON, C.E. (2010). Analytical Chemistry 39(3), 184-190.

Patterson, B.M. et. al., (2011), Microscopy and Microanalysis, submitted 12/10.

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