Existing Microbeam Facilities

1. Existing Microbeam Facilities I.C. Noyan IBM Research Division, Yorktown Heights. Dept. of Appl. Phys. & Appl. Math. Columbia University

2. Microbeam facilities exist in all major synchrotrons. • I will discuss the capabilities of: • Spring-8 • ESRF • APS • ALS • CHESS

3. Normal x-section ~ l Oblique X-section Important Parameters • Beam size on sample • Not necessarily equal • to the beam size at focus point. • Divergence • These terms may differ in vertical and horizontal directions. • # 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.

4. The data shown are either from the web pages 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.

5. SPring-8 (Super Photon ring-8 GeV) http://www.spring8.or.jp/ENGLISH/

6. Industrial Consortium ID (13 companies) BL16XU Undulator 4.5 - 40 keV X-ray diffraction, X-ray fluorescence analysis and X-ray microbeam analysis for characterization of new industrial materials. Industrial Consortium BM (13 companies) BL16B2 Bending Magnet 3.5 - 60 keV XAFS and X-ray topography for characterization of new industrial materials. Hyogo(Hyogo Prefecture) BL24XU Undulator 3.5 - 60 keV Protein crystal structure analysis. Surface/interface analysis of inorganic materials. X-ray microbeam analysis. X-ray imaging.

7. BL24XU-Hyogo Beamline: • Figure-8 undulator, vertically polarized X-ray beam. • Vertical axis double crystal monochromator • Beam 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 100 surface crystals. • Beam size @ sample: 7.3 mm x 6.4 mm (horizontal/vertical), • Beam divergence @ sample: 7.7/5.3 mrad

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

9. ESRF-The European Synchrotron RadiationFacility Grenoble, France http://www.esrf.fr

10. µ-FID :Micro-Fluorescence, Imaging and Diffraction, http://www.esrf.fr/exp_facilities/ID22/ • Optics • Flat Si mirror with 2 coatings • Horizontal deflection: 0.15º (2.6 mrad) • Cut-off energies: • Si strip: 12 keV • Pd strip: 24 keV • Pt strip: 32 keV • Vertical 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] crystals • Micro-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.

11. Detectors: • Si(Li) detector • Si drift diode detector • PIN diodes, ionization chambers • High resolution CCD cameras • Medium resolution CCD camera • gas filled (position sensitive) detector • Beam: • Monochromatic (4-35 keV), • PINK beam mode: High energy bandwidth beams obtained directly from the undulator and mirror. These beams span several full undulator harmonics.

12. 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 a high/medium resolution CCD camera stage. • A 6 circle diffractometer, featuring a 3 mm sphere of confusion is installed in the first experimental 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 microscope for alignment. • Typical distance between the beam path and the surface of the tableis 38 cm. The experiment is currently operated in air but special sample chambers can be mounted for in vacuum measurements.

13. General Description of ID18F Schematic lay-out of the ID18 beam-line and the ID18F user end-station

14. 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 for creating 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.

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

17. Imaging and tomography • Phase-contrast imaging: • Phase-contrast images of dry and wet samples can be taken on high-resolution film or by means 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 parallel beam, 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 to observe details of the very fine topography of exotic or modified crystals used in microelectronics or laser technology • Holography and interferometry: • Gabor in-line holography (planar reference wave) or Fourrier holography (spherical reference wave) are feasible. The fine interference pattern obtained can be used for the high accuracy determination of optical density and refraction index.

18. 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 inner structure of the fiber

19. Beamline ID13 The principal aim of the Microfocus Beamline is to provide small focal spots for diffraction and small-angle X-ray scattering (SAXS). Both single crystal and scanning diffraction (SXD) experiments are performed. Other applications, like scanning X-ray microfluorescence (SXRF), are feasible. http://www.esrf.fr/exp_facilities/ID13/

21. 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 based on a condensing mirror and collimators. • The scanning setup was developed for wide- and small-angle scattering. Typical beam sizes used are currently 2/5/10 mm based on a condensing mirror in combination with tapered glass capillaries or collimators. • The scanning setup can also be used for SAXS-experiments. For a beam size of about 10 mm, the first order spacing of dry collagen can be resolved (65 nm). A 130 mm entrance window MAR CCD with 16 bit readout (~ 4 sec readout/frame) or a XIDIS detector with 12 bit readout (~ 0.1 sec readout/frame) are used for scanning.

22. X-rays are guided inside the • capillaries by total external • reflection. • Critical angle depends on • material and l. ~0.1-10 mrad. • Capillaries tend to be very • long (many cm) with a small • slope. • 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

23. Advanced Photon Source Argonne, IL http://www.aps.anl.gov/

24. Sector 2: Micro-Techniques Group • High-resolution imaging and diffraction experiments in the • 1-4 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.

25. Fresnel zone plate: A circularly symmetric array of • annular zones which are alternately • transparent and opaque. • Provide diffraction limited x-ray imaging • with 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.

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

28. 2-ID-D - Sector 2, Insertion Device Branch Beamline High-resolution fluorescence and diffraction imaging, 

31. Optical micrograph. Strain effects Small beams are needed.

32. 2-ID-E - Sector 2, Insertion Side Device Branch Beamline Sub-micron x-ray fluorescence mapping: Detector: 3-element energy-dispersive, DE = 160 eV

33. 2-ID-B - Sector 2, Insertion Device Branch Beamline High-resolution imaging, Coherent scattering

34. devices devices devices 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 end of the aluminum interconnect shown in the right side in Fig. 3. 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). The last two years has seen an improvement in both spatial resolution an overall image quality in the tomography of integrated circuit components at beamline 2-ID-B. In collaboration primarily with a research group at the National Institute of Standards and Technology, we have been developing tomographic imaging techniques capable of resolving sub-micron sized structures, hence the name

35. 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.

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

37. ALS-Berkeley Lab, Berkeley, CA http://www-als.lbl.gov/

41. 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/

42. Summary • There are quite exciting machines that are doing microbeam x-ray analysis. • This is a hot area: • ESRF now reports microbeam results as a separate category. • All have advantages and limitations. • Ease of access, • Multiple techniques with minimal set-up. • New rings are being designed with microspot beamlines.

43. Diamondwill be built at the Rutherford Appleton Laboratory and is due to be available to 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 0.7Å – 1.3Å • Bandpass 10-4 • Convergence Up to 2mrad • Energy stability 0.25eV • Beamsize at sample 5 – 100m • Positional stability 1% RMS on 5s timescale • 3% RMS on 1hr timescale • Flux 1012 ph/s in 30m x 30m @ 1Å

44. Goniostat: Single axis with 1m 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 and simultaneous analysis capabilities not available at other machines.