characterization of target materials using a variety of x ... · characterization of target...

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Characterization of Target Materials Using a

Variety of X-ray Instrumentation

Brian M. Patterson, Kevin Henderson, Tana Cardenas, Derek

Schmidt, John Oertel, Matthew Herman, Joseph Cowan, Ted

Baumann

LAUR:17-21853


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▪ Several types of X-ray instrumentation is used to characterize target

materials, targets, as well as novel structures.

▪ Quantification for structure and density are routinely practiced.

▪ Demonstrated examples:

– Monochromatic radiography to measure the density of aerogels

– 3D tomography to characterize foam morphology

– 3D tomography to image novel structures and inclusions on

various size scales.

Applications

Slide 2


UNCLASSIFIEDSlide 3

LANL’s Density Characterization

Station▪ 10-3 Torr

▪ Doubly Curved Ge Crystal

▪ 13.2 μm pixel pitch

▪ FOV = ~9 mm x ~27.5 mm

▪ Three systems

– Mo = 2.3 keV

– Cr = 5.414 keV

– Cu = 8.047 keVGain 2; 2MHz readout frequency

Low noise readout

1.36 sec exposure time

250 Accumulations

10 Accumulation dark current subtraction


UNCLASSIFIEDSlide 4

• Density (ρ) is calculated using the following equation:

ρ =−ln𝑇 ν0𝐾 ν0 𝑧

Where:

T (ν0) = transmittance at frequency ν0 , = I/ I0

ν0 = frequency of monochromatic X-ray source

K (ν0) = opacity at frequency ν0, cm2 g-1

z = depth (thickness of sample), cm

Lanier, N. E.; Hamilton, C.; Taccetti, J. M. Review of Scientific Instruments 2012, 83, 10E521.

LANL’s Density Characterization

Station


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keV distribution

Slide 5

0 2 4 6 8 10

2

4

6

8

10

12

Y lo

ca

tio

n (

mm

)

X location (mm)

0.3900

0.3915

0.3930

0.3945

0.3960

0.3975

0.3990

0.4005

0.4020

Transmittance

The keV energy variation over the central 1 cm2, is ~0.001 transmittance.


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Analysis of 20 mg/cm3 aerogels.

▪ Right circular cylinders were made by LANL and

LLNL, targeting 20 mg/cm3.

▪ LANL’s Cu-based Density Characterization Station

was used to image the samples, operating at 8.04

keV (Cu Kα)

▪ Samples were also measured for density,

gravimetrically.


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Samples AA,AB▪ 10 mm-thick silica aerogel imaged with Cu-based

DCS @ 8.04 keV

▪ ROIs analyzed are indicated by yellow outline

SiO2 Aerogel AA

(ROI 1)

SiO2 Aerogel AB

(ROI 2)

Measured Density

(mode, mg cm-3) 21.6 21.1

Target Density

(mg cm-3)20 20

Measured

% Transmission

(mode)

50.3 50.8

Target

% Transmission53.0 52.7


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Samples CA,CB▪ 10 mm-thick silica aerogel imaged with Cu-based

DCS @ 8.04 keV


SiO2 Aerogel CA

(ROI 1)

SiO2 Aerogel CB

(ROI 2)

Measured Density

(mode, mg cm-3) 29.5 30.1

Target Density

(mg cm-3)20 20

Measured

% Transmission

(mode)

38.8 38.2

Target



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Samples DA,DB▪ 10 mm-thick silica aerogel imaged with Cu-based

DCS @ 8.04 keV


SiO2 Aerogel DA

(ROI 1)

SiO2 Aerogel DB

(ROI 2)

Measured Density

(mode, mg cm-3) 34.1 30.8

Target Density

(mg cm-3)20 20

Measured

% Transmission

(mode)

35.4 38.0

Target



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Samples EA,EB▪ 10 mm-thick silica aerogel imaged with Cu-based

DCS @ 8.04 keV


SiO2 Aerogel EA

(ROI 1)

SiO2 Aerogel EB

(ROI 2)

Measured Density

(mode, mg cm-3) 29.1 28.9

Target Density

(mg cm-3)20 20

Measured

% Transmission

(mode)

39.5 40.1

Target



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Samples FA,FB▪ 10 mm-thick silica aerogel imaged with Cu-based

DCS @ 8.04 keV


SiO2 Aerogel FA

(ROI 1)

SiO2 Aerogel FB

(ROI 2)

Measured Density

(mode, mg cm-3) 28.3 28.9

Target Density

(mg cm-3)20 20

Measured

% Transmission

(mode)

40.8 40.2

Target



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Samples LANL: 1 & 2▪ 3 mm-thick silica aerogel imaged with Cu-based

DCS @ 8.04 keV


SiO2 Aerogel

(ROI 1)

SiO2 Aerogel

(ROI 2)

Measured Density

(mode, mg cm-3) 24.0 21.7

Target Density

(mg cm-3)20 20

Measured

% Transmission

(mode)

75.2 74.5

Target



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DCS @ 8.04 keV


SiO2 Aerogel

(ROI 3)

SiO2 Aerogel

(ROI 4)

Measured Density

(mode, mg cm-3) 18.6 23.6

Target Density

(mg cm-3)20 20

Measured

% Transmission

(mode)

76.2 75.2

Target



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DCS @ 8.04 keV


SiO2 Aerogel

(ROI 5)

SiO2 Aerogel

(ROI 6)

Measured Density

(mode, mg cm-3) 23.0 26.6

Target Density

(mg cm-3)20 20

Measured

% Transmission

(mode)

72.4 72.7

Target



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Summary

Samples

Average Measured

Density

(DCS, mg cm-3)A,B

Average Measured

Density

(DCS, mg cm-3)A,C

Average Measured

Density

(Gravimetric, mg cm-3)A

LLNL 26.1 ± 3.4 28.2 ± 4.0 30.7 ± 0.56

LANL 28.9 ± 2.0 22.9 ± 1.5 22.0 ± 0.68D

A Errors are standard deviations of the average for the many samples.B Measured density using the mold size as the X-ray path lengthC Measured density using the true thickness of the sample as the X-ray path lengthD LANL aerogels were too light to measure individually, therefore 14 of them were weighed together to

produce an average mass.


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Micro/Nano CT Laboratory


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Xradia Micro Computed TomographyX-ray Source: Micro Focus Hamamatsu 5 m spot, 40

– 150 kV acceleration voltage, 10 W total power (4W

nominal)

Detector: 2k x 2k Electrically Cooled CCD, 4

objectives

Available Objectives:

2X 6 m/ pixel, 12 mm FOV

4X 3 m/ pixel, 6 mm FOV

10 X 1.2 m/ pixel, 2.4 mm FOV

20X 0.6 m/ pixel, 1.2 mm FOV (1.5 m resolution)

In-situ studies:

Sample may be imaged in states of either

tension or compression

Dynamic changes can be tracked in 3D


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Xradia UltraXRMLarge FOV = 65 µm, 150 nm resolution

Small FOV = 15 µm, 50 nm resolution

Absorption or Zernike phase contrast


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X-ray micro-scale imaging of marble capsules

Three DVB foam filled capsules were received and imaged using micro tomography

Sample ID’s Include:

Omega-Marble 16A 90 µm pore CHCD#26

Omega-Marble 16A 50 µm pore CHCD #15


Glass capsules are used as the pore former and are then etched out, leaving the pore

structure behind.

Physicists need to know the void size and distribution within the capsules; to get the

experimental pre-mix conditions.

Samples were imaged using Micro CT:

20X objective, 1 mm field of view, 1.07 µm voxel size, 40 kVp,

10W


UNCLASSIFIEDSlide 20


0

100

200

300

400

500

600

0 20 40 60

Occu

ren

ces

Equivalent Diameter (micrometers)

27 µm average void diameter

59.7% void volume




0

20

40

60

80

100

120

140

160

0 20 40 60

Occu

ren

ces


44 µm average void diameter

54.4% void volume



Omega-Marble 16A 90 µm pore CHCD#26

93.7 µm average void diameter

59.2% void volume

0

2

4

6

8

10

12

14

16

0 20 40 60 80 100 120

Occu

ran

ces



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3D printed capsule with microlatticeCharacterization of 3D printed capsule, 300 micrometers in diameter, with an interior

hexagonal microlattice using Nanoscribe 2PP instrument.

Physicists want better control and flexibility over the structure within the capsule

(see previous slides). Near zero density material for suspending inner capsules with

respect to double-shell design.



Imaged using SEM (electron microscope) and Micro CT (X-ray computed tomography)

Micro CT system was operated at:

20X magnification, 40kVp, 10 W, 1.0 micrometer voxel size.

Optical photo of capsule.

Rendering of

CAD file

Measurements


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Electron microscope images of the capsule

- Lattice ligaments are approximately 2 micrometers in diameter


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CT rendering of capsule

Ligaments are ~1.5

micrometers

in diameter

CT voxel size is ~1 micrometers

Therefore the ligaments were

also imaged and rendered using

nano-scale CT.


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Results:

The capsule printed with the interior hexagonal lattice.

Lattice is connected to the interior wall of the capsule.

A wedge was left out of the capsule wall to ease in the removal of the printing

fluid.

Capsule was probably ‘squished’ a bit as a result of handling. Some of the

ligaments are deformed and there is a flat area of the outer wall.

Ligaments are 1-2 micrometers in thickness; this is below the resolution of the

micro-CT. A 3D image of the capsule is currently underway using the nano-CT

instrument.


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Rochester sent us a cryogenic capsule to image some features that they were

seeing optically.

The capsule was received and mounted on a flattened tip of a finishing nail

using UV curable glue.

The capsule was imaged initially with an Xradia (Carl Zeiss X-ray Microscopy

Inc.) micro CT using the 20X objective. Nominal voxel size of 1 micrometer.

This was used to image the entire capsule.

Several images were collected of the capsule using our Xradia Ultra XRM.

High resolution, phase contrast modality; 15 micrometer FOV, 15 nanometer

voxel size.

The spot of interest is less than 0.5 micrometers in size and could not be

located in normal absorption contrast. It is within the wall of the sample. (It

may be a trapped air bubble??) Two surface contaminants were also identified

and imaged separately.

Nano-scale CT of a cryogenic capsule


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Optical images (Zeiss) of the

capsule showing locations of

glue surrounding a point of

concern, or spot. Respective

Nano CT locations are also

provided.

spot

CT spot 1

glueUniversity of Rochester

optical (Leica) map of region

with spot.

spot

CT spot 2

Optical Images


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Micro CT reconstructions of the complete

capsule. At this resolution, no features of

the spot can be recognized. CT spots 1

and 2 can be easily detected.

CT spot 2

CT spot 1

CT spot 1


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Nano CT HRES reconstruction of the region of interest at the spot between the three

daps of glue. The spot is located on the inner surface of the capsule and is about ~0.5

µm in size.

xy plane

xz plane

yz plane

Shell thickness ~5.8 µm

spot

Inner surface

Outer surface

spot

spot


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Nano CT HRES reconstruction of the region of interest at CT spot 1. The spot is

located on the outer surface of the capsule and is about ~ 2 - 4 µm in size.

3D Rendering

xy plane

HRES

xy plane

HRES

xz plane

yz plane


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Nano CT HRES reconstruction of the region of interest at CT spot 2. The spot is

located on the outer surface of the capsule and is also about ~ 3 - 5 µm in size. HRES

xy plane

HRES

xz plane

xy plane xz plane


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Conclusions:

LANL uses a variety of X-ray instruments (confocal XRF will be shown in the

poster) to characterize target materials, targets (see Tana’s talk), novel

designs, and defects.

Monochromatic radiography is used to measure the density of low density

materials as well as thin films (not shown today). This technique also provides

2D radiographs that can filter out samples that may meet the density

specification, but have other issues.

Micro CT is used to measure void size, shape and distribution, providing the

physicists a true understanding of the as-shot material.

Nano CT is used to image smaller features and defects.

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