Ce v Microbeam Lines

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Existing Microbeam Facilities

I.C. Noyan

IBM Research Division,

Yorktown Heights.

Dept. of Appl. Phys. & Appl. Math.

Columbia University


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Microbeam facilities exist in all majorsynchrotrons.

I will discuss the capabilities of: Spring-8 ESRF

APS ALS CHESS


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Important Parameters

Beam size on sample Not necessarily equal

to the beam size at focus point.

Divergence

These terms may differ in vertical and horizontaldirections.

# of photons in beam (intensity) Divergence, beam intensity and the scattering process must be

evaluated together.

Only the photons within the acceptance aperture of the process are

relevant.

~l

Normalx-section

ObliqueX-section


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The data shown are either from the webpages or publications as of 1/2003. The URL for each institution is referenced

once at the beginning of each section.

Other data is referenced as required.


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SPring-8 (Super Photon ring-8 GeV)

http://www.spring8.or.jp/ENGLISH/


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Industrial Consortium

ID (13 companies)

BL16

XU Undulator

4.5 -

40keV

X-ray diffraction, X-ray fluorescenceanalysis and X-ray microbeam

analysis for characterization of newindustrial materials.

Industrial ConsortiumBM (13 companies)

BL16

B2

Bending

Magnet

3.5 -60

keV

XAFS and X-ray topography forcharacterization of new industrial

materials.

Hyogo(Hyogo Prefecture)

BL24XU

Undulator3.5 -60keV

Protein crystal structure analysis.Surface/interface analysis of inorganicmaterials. X-ray microbeam analysis.X-ray imaging.


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BL24XU-Hyogo Beamline:Figure-8 undulator, vertically polarized X-ray beam.Vertical axis double crystal monochromatorBeam size 100 mm x 60 mm at limiting slit (65 m from source)Horizontal/vertical divergence: 16/1 mrad @ slit.Condensing optic: Asymmetric reflection (511 + -) from 100surface crystals.

Beam size @ sample: 7.3 mm x 6.4 mm (horizontal/vertical),Beam divergence @ sample: 7.7/5.3 mrad


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Kimura, et. al., APL Vol.77 #9, pp. 1286-1288 (2000)


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ESRF-The European

SynchrotronRadiationFacility

Grenoble, Francehttp://www.esrf.fr


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OpticsFlat Si mirror with 2 coatings

Horizontal deflection: 0.15 (2.6 mrad)Cut-off energies:Si strip: 12 keV

Pd strip: 24 keVPt strip: 32 keVVertical double flat crystal monochromator, fixed exit cam system (Kohzu)

Angular range: 3-30 deg.Energy range:4-37 keV for Si[111] crystals

7-72 keV for Si[311] crystalsMicro-focusing elements:Bragg-Fresnel lenses (BFL)Fresnel zone plates (FZP)Compound refractive lenses (CRL)

Size of beam at the sample location (V x H): 0.85 mm x 1.5 mm @ 40 m (EH1) and 1.2 x 2.2 @

60 m (EH2). 109, 1012 photons/sec.@ sample.

-FID :Micro-Fluorescence, Imaging and Diffraction,

http://www.esrf.fr/exp_facilities/ID22/


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Detectors:

Si(Li) detector

Si drift diode detector

PIN diodes, ionization chambersHigh resolution CCD cameras

Medium resolution CCD camera

gas filled (position sensitive) detector

Beam:

Monochromatic (4-35 keV),

PINKbeam mode: High energy bandwidth beams obtained directly from theundulator and mirror. These beams span several full undulator harmonics.

E d St ti


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End Station

Two large experimental hutches (~30m2 each) accept differentset-ups:The microprobe facility: on a 2.5 x 1.2 m 2 granite optical table.

focusing stage,pinhole stage,

sample scanning stage with 2 sample holders (goniohead or slide holder)Video microscope, fluorescence, diffraction and normalization detectors as well as ahigh/medium resolution CCD camera stage.A 6 circle diffractometer, featuring a 3 mm sphere of confusion is installed in the firstexperimental hutch and is operated jointly with the Univ. of Karlsruhe.

The imaging and tomography set-up: second hutch, includes a high resolution rotation

sample stage, a CCD X-ray camera standing on an optical bench and an optical microscopefor alignment.Typical distance between the beam path and the surface of the tableis 38 cm. The experiment iscurrently operated in air but special sample chambers can be mounted for in vacuummeasurements.


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Schematic lay-out of the ID18 beam-line and the ID18F user end-station
http://www.esrf.fr/exp_facilities/ID22/ID18F/id18fendst.html


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The microprobe set-up is situated on a movable granite table in the 3rd hutch of the ID18 beamline at

about 59 m distance from the X-ray source. For the demagnification of the synchrotron source and forcreating the micro-beam, parabolic compound refractive lens (CRL) is used. The CRL] is composed of

different number of individual Al lenses depending on the energy of the focused beam. The typical focal

distance is between 0.5-1.2 m depending on the energy of the incoming beam leaving a relatively large

place between the sample and focusing device for placing e.g. beam-shaping (pin-hole) or beam

monitoring (photodiode, ionization chamber) elements in between.
http://www.esrf.fr/exp_facilities/ID22/ID18F/id18fendst.html


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The size of the focused beam is typically 1-2 micron vertically and 12-15 micron horizontally


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Imaging and tomography

Phase-contrast imaging:Phase-contrast images of dry and wet samples can be taken on high-resolution film or bymeans of a high-resolution CCD camera. Typical exposure times are 10 ms to 5 s.

Phase-contrast microtomography:Collecting a set of phase contrast images from different orientations of a sample in a parallelbeam, it is already possible to perform 3D reconstruction (back-projection algorithm) by

tomography at the micrometer scale.Micro-topography:,

The high contrast and high resolution achievable is be used on the micro-FID beamline toobserve details of the very fine topography of exotic or modified crystals used inmicroelectronics or laser technology

Holography and interferometry:

Gabor in-line holography (planar reference wave) or Fourrier holography (sphericalreference wave) are feasible. The fine interference pattern obtained can be used for the highaccuracy determination of optical density and refraction index.


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Boron fiber

reconstructed cross-section through a 100 micron boron fiber with a 15 micron tungsten-borite core,reconstructed from 700 phase-contrast images in 5 cm recording distance (E=20 keV)Three dimensional visualization of the broken tip of the fiber. A block has been cut out to show the innerstructure of the fiber
http://www.esrf.fr/exp_facilities/ID22/tomo.html


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BeamlineID13

The principal aim of theMicrofocus Beamline is toprovide small focal spots for diffraction and small-angle X-ray scattering (SAXS). Both single crystaland scanning diffraction (SXD) experiments areperformed. Other applications, like scanning X-raymicrofluorescence (SXRF), are feasible.

http://www.esrf.fr/exp_facilities/ID13/
http://www.esrf.fr/http://www.esrf.fr/


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http://localhost/var/www/apps/conversion/tmp/scratch_4/machine_homepage.htmhttp://localhost/var/www/apps/conversion/tmp/scratch_4/optical_pic.htmhttp://localhost/var/www/apps/conversion/tmp/scratch_4/huch1_pic.htmhttp://localhost/var/www/apps/conversion/tmp/scratch_4/hutch2_pic.htmhttp://www.kagaku.com/kohzu/english.htmlhttp://localhost/var/www/apps/conversion/tmp/scratch_4/mirror_tab.htmhttp://localhost/var/www/apps/conversion/tmp/scratch_4/capillary_page.htm


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The main instrumental setups available for users are:

The microgoniometer was developed for protein crystallography(PX) but can also be used for small- to medium cell

crystallography. Typical beam sizes available are 5/10/30 mm basedon a condensing mirror and collimators.

The scanning setup was developed for wide- and small-anglescattering. Typical beam sizes used are currently 2/5/10 mm basedon a condensing mirror in combination with tapered glasscapillaries or collimators.

The scanning setup can also be used for SAXS-experiments. Fora beam size of about 10 mm, the first order spacing of dry collagencan be resolved (65 nm). A 130 mm entrance window MAR CCD

with 16 bit readout (~ 4 sec readout/frame) or a XIDIS detectorwith 12 bit readout (~ 0.1 sec readout/frame) are used for scanning.


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X-rays are guided inside thecapillaries by total externalreflection.

Critical angle depends onmaterial and l. ~0.1-10 mrad.

Capillaries tend to be verylong (many cm) with a smallslope.

Usually 1 to 3 reflections.Non-imaging optic.

Material: Pb-glass, r=5.3 g/cm3,Att. Length ~ 40 mm @12 keV, qcrit~3 mrad.

http://www-hasylab.desy.de/science/groups/syxrf/capillar.html


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Advanced Photon Source

Argonne, IL

http://www.aps.anl.gov/


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Sector 2: Micro-Techniques Group

High-resolution imaging and diffraction experiments in the1-4 keV and 5-35 keV energy regions.

Develop new x-ray optics and techniques, with an emphasis

on nanofocusing, coherence, 3D, and high-throughput methods.

F l l t A i l l t i f


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Fresnel zone plate: A circularly symmetric array of

annular zones which are alternately

transparent and opaque.

Provide diffraction limited x-ray imagingwith a spatial resolution (in first order)

approaching the dimension of the

minimum, i.e., outermost, zone width.

Provides many imaging orders.

Different orders are focused at different

points.

Monochromatic and spatially coherent

illumination of the zone plate is required

in order to get a diffraction-limited

focal spot size.


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http://xuv.byu.edu/html/docs/previous_research/EUV_Imager/Documentation/part4/4fresnel.htm


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Energy Range

Monochromaticity

2.0-32.0 keV

104 E/dE

Beam size 4.2 x 1.6 mm2 (hor x vert) FWHM

Microprobe focussize 0.1 x 0.1 um2 (hor x vert)

Microprobe flux 1011 ph/um2/s/0.1% BW

2-ID-D - Sector 2, Insertion Device Branch Beamline

High-resolution fluorescence and diffraction imaging,


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Optical micrograph.

Strain effects

Small beams are needed.


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Energy range 8.0 - 12.5 keV

Monochromaticity 104 E/DE

Beam size2.0 x 1.0 mm2 (hor x vert)

FWHMMicroprobe focus

size0.3 x 0.3 um2 (hor x vert)

Microprobe flux 1011 ph/um2/s/0.1% BW

2-ID-E - Sector 2, Insertion Side Device Branch Beamline

Sub-micron x-ray fluorescence mapping:

Detector: 3-element energy-dispersive, DE = 160 eV


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2-ID-B - Sector 2, Insertion Device Branch Beamline

High-resolution imaging, Coherent scattering

Energy range 0.5 - 4.0 keVMonochromaticity 102 - 104 E/dE

Beam size 350 x 150 um2 (hor x vert) FWHM

Nanoprobe focus size 50 x 50 nm2 (hor x vert)

Nanoprobe flux 107 - 108 ph/s/0.1% BW

Absolute-calibrated photodiodesAvalanche photodiodesDispersive LEGe fluorescence detector

LN2-cooled CCD cameras (direct, scintillator)Fast scan stage (0.8 nm resolution)


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Z. H. Levine, A.R. Kalukin, M. Kuhn, S.P. Frigo, I. McNulty, C.C. Retsch,

Y. Wang, U. Arp, T. Lucatorto, B. Ravel, C. Tarrio, J. Appl. Phys. 87, 4483 (2000).

1. A projective plot of the reconstruction

of the integrated circuit.

2. Bayesian reconstruction of the integrated

circuit interconnect using same data as in 1.

3. Normal incidence projection of an

integrated circuit interconnect with an

electromigration void.

4. Bayesian reconstruction of the ragged endof the aluminum interconnect shown

in the right side in Fig. 3.


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MHATT-CAT-Sector7 /UNICAT Beamline 34

White beam/monochromatic rad.

K-B mirrors

Spot size~1 micrometer diam.Divergence~2-4 mrad.

Grain by grain strain/texture mapping.

Depth resolved strain mapping.


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Sample geometry

G. Ice, B. Larson, Nature415, 887 - 890 (2002)


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ALS-Berkeley Lab, Berkeley, CA

http://www-als.lbl.gov/

Beamline 7.3.3 X-Ray Microdiffraction


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X Ray MicrodiffractionSourcecharacteristics

Bend magnet

Energy range 6-12 keV

Monochromator White light and monochromatic [two- and four-crystalGe(111)]

Calculated flux (1.9GeV, 400 mA)

At typically 8.5 keV:1 x 109 photons/s/m2/3x10-4BW (1 x 1 m spot), 1 x1012 photons/s/3x10-4BW (100 x 300 m spot)

Resolving power(E/DE)

1000-7000 depending on vertical convergenceaccepted

Detectors X-ray CCD, image plate, fluorescence Si(Li) detector

Spot size atsample

100 x 300 m down to 1 x 1 m

Samples

Format Typically less than 1 cm2 x 1 mm thick

Sampleenvironment

Typically air

Special notes Microprobe, white-light, and monochromaticexperiments

Scientific

applicationsMeasurement of thin film strain, environmental science

Beamline 6.1.2 High-Resolution Zone-Plate Microscopy


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g pySource characteristics

Bend magnet

Energy range300-900 eV

MonochromatorZone-plate linear

Calculated flux (1.9 GeV,400 mA) Images with 1000 x 1000 pixels, 1000 photons/pixel

recorded in 3 s at 517 eV, 0.2% BW

Resolving power (E/DE)500-700

Endstations X-ray microscope (XM-1)

Characteristics

Full-field soft x-ray microscopeSpatial resolution

25 nm

Detectors Back-thinned CCD camera

Field of view10 m single field; larger areas can be tiled togetherlike a mosaic

Beamline 10.3.1 X-Ray Fluorescence Microprobe


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y p

Sourcecharacteristics

Bend magnet

Energy range 6-15 keV (with multilayer mirrors)3-20 keV (without multilayer mirrors)

Monochromator White light, multilayer mirrors in Kirkpatrick-Baezconfiguration

Calculated flux

(1.9 GeV, 400 mA) 3 x 1010

photons/s at 12.5 keVResolving power(E/DE)

25 at 12.5 keV

Endstations Large hutch with optical table

Characteristics X-ray fluorescence analysis of samples with highelemental sensitivity and high spatial resolution

Spatialresolution

1.0 x 1.2 m

Detectors Si(Li)

Spot size atsample 1.0 x 1.2 m


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CHESS, Ithaca, NY

B2 bend magnet station,

Tapered capillary optic,Smallest beam: 1000 A diameter @ 6 keV.

106 photons/sec at the sample @ 12.3 keV

(multilayer mono.)

Microstructure evaluation (Laue photos).

http://www.chess.cornell.edu/


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Summary

There are quite exciting machines that are doingmicrobeam x-ray analysis.

This is a hot area:

ESRF now reports microbeam results as a separatecategory.

All have advantages and limitations.

Ease of access,

Multiple techniques with minimal set-up.

New rings are being designed with microspot beamlines.


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Diamondwill be built at the Rutherford Appleton Laboratory and is due to be availableto users in September 2006.

24 cells/ 3.0 GeV ring.Undulator beams up to 20keV

High flux from multipole wigglers and wavelength shifters to energies greater than 100keV.Bending magnet sources from 40 keV to the IR.Microbeamline:.

Source: undulator

Optics: double crystal monochromator with micro-focussing giving:

Wavelength range 0.7 1.3Bandpass 10-4Convergence Up to 2mradEnergy stability 0.25eV

Beamsize at sample 5 100mmPositional stability 1% RMS on 5s timescale

3% RMS on 1hr timescale

Flux 1012 ph/s in 30mm x 30mm @ 1


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Goniostat: Single axis with 1mm sphere of confusion,

Detectors:

Area detector with no more than 1s readout time;

Fluorescence detector

Auto-loading and auto-changing of sample.

Auto-alignment of sample both optically and with X-rays

Sample cryogenic cooling to 4 100K

The proposed machine at NSLS will provide ease-of-use andsimultaneous analysis capabilities not available at other machines.

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Ce v Microbeam Lines