Post on 04-Apr-2018
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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.html7/30/2019 Ce v Microbeam Lines
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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.html7/30/2019 Ce v Microbeam Lines
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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.html7/30/2019 Ce v Microbeam Lines
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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/7/30/2019 Ce v Microbeam Lines
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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.htm7/30/2019 Ce v Microbeam Lines
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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.