joe arkoadvanced photon source ralu divan kurt goetze tim mooney david paterson stefan vogt
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Soft X-ray Microscopy at the APS. Ian McNulty. Argonne National Laboratory. Wednesday, 9 October 2002. Many thanks to. Joe ArkoAdvanced Photon Source Ralu Divan Kurt Goetze Tim Mooney David Paterson Stefan Vogt Petr Ilinski Shenglan Xu Sean FrigoNorthern Arizona University - PowerPoint PPT PresentationTRANSCRIPT
Joe Arko Advanced Photon SourceRalu DivanKurt GoetzeTim MooneyDavid PatersonStefan VogtPetr IlinskiShenglan Xu
Sean Frigo Northern Arizona UniversityCornelia Retsch Saint-Gobain Sekurit DeutschlandNathan Krapf University of Chicago
Steve Wang Xradia CorporationWenbing Yun Xradia CorporationErik Anderson CXRO, Lawrence Berkeley National LaboratoryFranco Cerrina CXRL, University of Wisconsin at Madison
Many thanks to ...
Soft X-ray Microscopy at the APS
Ian McNulty
Argonne National Laboratory
Wednesday, 9 October 2002
APS
Summary
Motivation
APS efforts
Scanning microscopy
Flash methods
Future
APS
1-4 keV: access most of periodic table
K
L
M
M
APS
Materials science
• Nondestructive in situ imaging of buried structures
• Visible/electron-opaque samples, less charging than with electrons
• Contrast at K,L,M-edges in industrially important materials(AI, Si, Ti, Cu, Ga, Ge, As, Sm, Eu, Gd, W, Au, . . .)
• Study electromigration and fabrication defects in chip interconnects
Biology
• Better resolution than optical, less damage than electron microscopy
• Specimens can be initially living, wet, unstained, and in air
• Natural Na, Mg, P, S, Ca contrast in this energy range
Environmental science
• Study S in soils, fossil fuels, catalyst sulfidation, lubricants
• Chemical as well as elemental contrast
APS
1-4 keV x-rays: applications
APS
Soft x-ray microscopy at APS
Magnetic materials 4-ID-C (J. Freeland)
XANES PEEM
MCD, MLD PEEM, scanning (future)
Materials, biology 2-ID-B (D. Paterson)
Transmission scanning, holography, full-field
Fluorescence scanning
Tomography scanning
Microdiffraction scanning
APS
PEEM images provide direct map of chemical and magnetic structure
1 m x 1 m x 15 nm Conanodots on Al substrate(as dep., no field history)
Chemical map (Co bright)
Magnetic map (M bright)
1 m
Beam direction
PEEM optics
Co
Chemical and magnetic microscopy at 4-ID-C
J. Freeland, D. Keavney, R. Winarski (APS)J. Shi, W.C. Uhlig (Univ. Utah)
APS
2-ID-B intermediate-energy beamline
Monochromaticity ~500 typ., > 3000 peak
Coherent area 50 m 50 m
Coherent flux 2 105 ph/m2 /s/0.1% BW
Focused flux 4 107 ph/s/0.1% BW 50 nm spot2 108 ph/s/0.1% BW 150 nm spot
APS
Scanning x-ray microscope
rotation stage
coarse/fine scan stage
avalanche or PN junction photodiode
sample on support
order-sorting aperture
zone plate
coherent x-rays
VME crate and workstation
preamp and discriminator
Ge detector
APS
Zone Plates
MaterialRadiusCentral stop radiusZone thicknessFinest zone widthTransverse resolutionFocal length (1.83 keV)Depth of field ( " " )Meas. Efficiency ( " " )
Au Au Ni Ni38.5 40 45 49 - - - 20420 650 110 130100 50 45 40122 61 55 4911.4 5.9 6.0 5.872 18 15 1220 12 2.5 3.0
m µm nm nm nm mmm %
Sample Stage (XYZ)
Linear rangeLinear resolutionLinear velocityAngular rangeAngular resolutionMax scan speed
Coarse
2550023600.0010.1
Fine
0.10.8203600.140.1
2-ID-B SXM specifications
mmnmmm/sdegreesdegreesms/pixel
APS
Contrast of a 100-nm Al wire on 1 µm of Si
APS
STXM image at 1553 eV. Al interconnects becometransparent below Al 1s edge (1559 eV), whereas W vias joining interconnects still appear dense.
Elemental contrast in Al/W/Si chips
STXM images of two-level Al/W/Si test structureat 1563 eV. SiO2 substrate was thinned to ~5 µm.Sample courtesy of DEC.
Steve Grantham Nat'l Inst. of Standards and TechnologyZachary LevineAndy Kalukin SAICMarkus Kuhn Intel Corporation
APS
Scanning nanotomography of AI/W/Si chips
Z. Levine, et al., Appl. Phys. Lett. 74, 150 (1999)Z. Levine, et al., J. Appl. Phys. 87, 4483 (2000)
3D Bayesian reconstruction oftwo-level structure at 1750 eV
Normal-incidence scanof electromigration void
3D reconstruction of ragged end of void
5 µm 1 µm 500 nm
APS
Nanoscale metrology in Cu/W/polyimide chips
(a) Schematic side view of a two-level Cu/W test structure. (b) STXM image at normal incidence. (c) Elevated surface plot. Sample courtesy of IBM.
Comparison of various line scans through structure
X. Su, et al., Appl. Phys. Lett. 77, 3465 (2000)
APS
1-4 keV x-rays: biological applications
• Natural contrast for nuclear and mitochondrial DNA at K-edge of P (2149 eV)
• Probe cell ion transport and membrane permeability at K-edges of Na (1.09), Mg (1.28), K(3.82), Ca (4.04 keV)
• Co-locate lighter elements with trace metals mapped by hard x-ray microscopy, at higher resolution
• Study chemical speciation of important inorganic elements (Mg, Al, Si, Ca), e.g. in marine organisms
APS
Phosphorus XANES
P K fluorescence from NaPO4
P 1s absorption spectra
APS
Simultaneous transmission, fluorescence detection
Gd 3d5/2, 3d3/2Si 1s
APS
• Cell is transfected with TiO2-DNA nanocomposites
• DNA targets specific chromosomal region
• TiO2 photocleaves DNA strands upon illumination
• Potential use in gene therapy
5 m
2.2
0.0
g/cm2
5.8
0.0
g/cm2
TiO2-DNA nanocomposites in mammalian cells
ZnTi
Map Ti distribution using x-ray induced K
fluorescence, to quantify success rate ofTiO2-DNA transfection and visualize target
Affinity of transfected DNA to ribosomalDNA causes nanocomposites to localizeto the nucleolus
G. Woloschak, I. Moric, T. Paunesku, N. Stojicevic(Radiation Biology Dept., Northwestern Univ.)
APS
Phosphorous absorption imaging
10 µm 5 µm 5 µm
Mouse PC-12 cell(fixed, dried)
Cell nuclei, separated by centrifugation(fixed, dried)
Energy 2170 eV
Step size 50 nm
Dwell 10 ms
Scan time 20 min
APS
Energy-resolved fluorescence mapping
5 µm
Whole mouse PC-12 cell (fixed, dried)Detergent wash, ethidium bromide stain
Transmitted Na K Br L
2 µm
APS
Nuclear contrast with P fluorescence
P K Si K
5 µm
Energy 2200 eV
Step size 150 nm
Dwell 1 s/pixel
Scan time 4 h
APS
What about radiation damage?
APS
Flash imaging methods
• HolographyUse x-ray optics to form reference wave and object illumination
• Full-field imagingUse x-ray optics to magnify sample image
• Diffraction with phase retrievalX-ray optics useful but not required
APS
Quantitative phase contrast by holography
B. Allman, A. Barty, P. McMahon,K. Nugent, D. Paganin, J. Tiller(Dept. of Physics, Univ. Melbourne)
B. Allman, et al., JOSA A17, 1732 (2000)J. Tiller, Ph.D. Thesis, U. Melbourne (2001)
Hologram of ~1 µm Al sphereson 100 nm formvar membrane
Difference between twoholograms at different foci
Reconstructed phase
APS
Full-field phase imaging
B. Allman, et al., JOSA A17, 1732 (2000)
Full-field image of ~2 µm spider silk
Difference between in-focus, defocused images
Reconstructed phase
APS
Phase imaging of optical fiber
APS
Phase nanotomography of Si AFM tip
3D reconstructions of real part of refractive index of projections.(a, b) Horizontal slices through tip. (c) Vertical slice. (d-f) Volume renderings. Measured = 5.0 ± 0.5 x 10-5 , calculated = 5.1 x 10-5.
P. McMahon, et al., Opt. Commun., in press
APS
Future developments
• Scanning microscope– New ZP on order (50 nm outermost zone, 450 nm Au)– Multiple SDDs to increase fluorescence acceptance– 2K x 2K fly scans
• Extend quantitative phase imaging to ~50 nm level– Improve alignment for d/dz series– Solve twin-image problem with TIE– Determine limits on coherent flux required
• 2-ID-B beamline– Multilayer gratings on order
APS
Conclusions
• 1-4 keV region highly attractive for x-ray microscopy
• 2-ID-B SXM is a workhorse instrument at APS– 50 nm (2D), 150 nm (3D) resolution– simultaneous transmission and fluorescence– Goal: reach photon limits near ~10 µs/pixel (transmission)
~0.1 s/pixel (fluorescence)
• Developing holography, coherent full-field imaging– Obtain quantitative absolute phase– Applicable to flash x-ray sources Beat radiation damage problem!