Edge Radiation IR end-station at ESRF

Transcription

1 X-TIP Workshop Coupling of Synchrotron Radiation IR and X-rays with Tip based Scanning Probe Microscopies November 2005 Edge Radiation IR end-station at ESRF Jean Susini European Synchrotron Radiation Facility, BP220, F Grenoble Cedex, France

2 Outline X-ray microprobes Some examples IR end-station Synchrotron based IR-SNOM? M. Cotte (ESRF) M. Salomé (ESRF) R. Baker (ESRF) E. Gagliardini (ESRF) K. Scheidt (ESRF) P. Dumas (SOLEIL) O. Chubar (SOLEIL) N. Rochat (CEA) F. Bertin (CEA) A. Chabli (CEA) F. Comin (ESRF) M. Silveira (ESRF) N. Chevalier (UJF-CEA) S. Huant (UJF-CNRS)

3 ID21 X-ray microscopy ID22 Micro-FID 2.1 < E kev < < σ µm < 1 µ-xrf µ-imaging (2D) µ-xanes In vacuum / Air Micro-analysis platform Imaging group ID21-FTIR Infrared spectro-microscopy 2 < λ µm < 12 Diffraction limited (λ/2) 5.0 < E kev < < σ µm < 3 (< 100nm ) µ-xrf and µxrd µ-imaging (2D 3D) µ-xanes Air / He Dry N 2

4 Attributes of multi-kev XRM (2-30keV) X-ray Fluorescence Trace element detection & mapping Quantitative fluorescence analysis Micro-spectroscopy (XANES) Chemical state specificity Higher penetration Phase contrast Microscopy on thick samples Lower radiation damage (?) Larger focal lengths (> 20mm) Larger depth of focus (> 100µm) Space for sample environment 3D imaging Multi-modal approach Micro-Fluorescence Micro-diffraction 3D imaging Spectroscopies In-situ experiments controlled sample environment

5 Attributes of multi-kev XRM (2-30keV) X-ray Fluorescence Trace element detection & mapping Quantitative fluorescence analysis Micro-spectroscopy (XANES) Chemical state specificity Higher penetration Phase contrast Microscopy on thick samples Lower radiation damage (?) Larger focal lengths (> 20mm) Larger depth of focus (> 100µm) Space for sample environment 3D imaging Multi-modal approach Micro-Fluorescence Micro-diffraction 3D imaging Spectroscopies In-situ experiments controlled sample environment

6 Imaging and micro-spectroscopy beamlines ID21-FTIR ID21 ID KeV 100 Sample raster scanned CCD Diffraction Crystal monochromator X-ray lens Photodiode Undulator CCD Alignment & imaging Fluorescence detector

7 Several signals and information available 1.0 Spectrum UO 2 U 3 O 7 particle1, (U, Pu)O 2 particle2, (XANES) UO 2 with U 'appauvri' Tomography - Absorption Trace element imaging - Fluorescence lni 0 /I, arb. units Energy, kev Diffraction

8 Science at ID21 and ID22/ID18F Materials Science 11% Archeometry 18% Instrumentation 2% Chemistry 8% Biology 7% Environ. Sciences 28% Bio-Medical 6% Geochemistry 17% Period: : > 210 experiments

9 Need for trace element analysis in heterogeneous systems Biology & Medicine Geochemistry & Earth Sciences Environmental Sciences Material sciences Quantification Redox reactions are monitored by Trace elements (metals) Co-localisation Oxydation states chemical speciation XANES detection and quantification X-ray fluorescence element co-localisation: 2D/3D mapping

10 Need for complementary techniques C, H, O, N Mg, Na, S, P, Cl, Ca, V, Cr, Fe, Cu, Zn, IR spectro-microscopy resolution + detection limit + chemical selectivity +++ functional groups X-ray spectro-microscopy resolution +++ detection limit (fluorescence) +++ chemical selectivity (XANES) +++ oxidation states

11 Synchrotron source: brightness advantage BRIGHTNESS Photons/sec/0.1%bw/mm 2 /str Synchrotron Radiation Universal Equation Practical limits 2000K Black Body Wavelength (microns) BROADBAND Signal-to-Noise Data Collection Spatial Resolution Spectro-microscopy Chemical mapping Spectroscopy

12 Two main modes of infrared emission 10 µm Bending magnet emission 10 µm Edge emission

13 ID21 FTIR Microscopy end-station: Combined studies with X-ray microscopy Compatibility with X-ray microscope sample holder Enlarge the palette of micro-analysis techniques available at the ESRF A unique facility for a coordinated use of IR and X-ray microscopes (physically close) a clear demand from the user s community: Archaeology, Environmental sciences, Earth sciences, Biology, Polymers, Cosmology stimulate the in-house research programme by developing a new culture IR+X-rays high potential for industrial applications

14 Various calcium sites in human hair shaft C. Merigoux et al., (a.u.) 30 µm cuticle Ca - XRF 0.2x0.2µm Wavenumbers (cm -1 ) Infrared Spectra

15 Various calcium sites in human hair shaft C. Merigoux et al., (a.u.) 30 µm cuticle Two different «types» of lipids in cuticule and medulla Ca - XRF 200x200nm 2 Protein distribution in cortex

16 ID21 Infrared microscopy end-station transfer line Edge radiation microscope spectrometer mirror-box

17 ID21 Infrared microscopy end-station transfer line Edge radiation microscope spectrometer mirror-box

18 Extracting mirror (K.Scheidt, DIPAC'05, June 2005) 6mm X-rays 72% - 10µm flat un-cooled aluminium mirror, with a 5mm horizontal slot. lets the energetic part of the synchrotron light go through the optic without heating it. vertically movable, centered on the heart of the X-ray beam in a slow feed-back loop by the use of thermo-probes. slotted mirror with 6mm vertical slot

19 Slotted extraction mirror Beam profile at 3.2m from entrance main dipole Absorbed power: 1.5KW a few watts 20mm λ=100µm 20mm λ=10µm Vertical Position Vertical Position mm Horizontal Position λ=50µm λ=1µm -30mm Horizontal Position

20 ID21 Infrared microscopy end-station transfer line Edge radiation microscope spectrometer mirror-box

21 The infrared end-station Microscope focuses the beam on the sample collects and detects the transmitted or reflected beam Spectrometer creates interferograms Computer Fourier Transform Data processing

22 Inside the microscope Confocal microscope: Two confocal Schwarzschild objectives: focus the light onto the sample collect the light and relay it to the detector. Diffraction-limited resolution of λ/2 ( λ: 2 12µm) G.L. Carr, Rev. of Scientific Instruments, 2001, 72, 1613

23 ID21 Infrared microscopy end-station transfer line user Edge radiation microscope spectrometer mirror-box

24 ID21-IR: Optical pathway M3 Toroidal M7 Elliptical M8a Parabolic M1 M2 M4 M5 M6 BM window diamond window KBr Interferometer & Microscope 3.m 2.55m 2.45m 2.473m 3.60m 0.50m 0.22m 2.40m 0.50m 0.08m

25 SRW code computations at 10 µm 10 mm 3 mm 5 mm 10 mm 3 mm 5 mm Measured intensity maps (integrated from 2 to 12 µm)

26 Synchrotron vs Globar ID21-IR Iintensity ratio Aperture (µm) Synchrotron Peak to peak intensity (V) Synchrotron Globar Aperture (µm) Globar 6 6 µm µm 2

27 Diffraction limit: long wavelength vs lateral resolution Log(1/R) µm 6µm 7µm 8µm 9µm 10µm 5µm 6µm 7µm 8µm 9µm 10µm Synchrotron radiation Globar ? Wave-numbers (cm -1 ) synchrotron globar 5 µm 15 µm

28 6/12/2004 Synchrotron based IR-SNOM? F. Bertin (CEA) R. Casalegno (SPECTRO) A. Chabli ( CEA) F. Comin (ESRF) M. Cotte (SPECTRO) P. Dumas (SOLEIL) M. Faucher (CEA) E. Garcia-Caurel (EP) S. Huant (SPECTRO) R. Ossikovski (EP) C. Rambaud (SPECTRO) N. Rochat (CEA) P. Royer (LNIO) J. Susini (ESRF) JJ. Yon (CEA) P. Chaton (CEA) JM. Ortega (CLIO) B. Drevillon (EP) Source? Illumination? Collection? Excitation? Detection? Diapason? Aperture? Modeling? Prototype with diapason Feasibility tests at ID21 N. Rochat (CEA) F. Bertin (CEA) A. Chabli (CEA) F. Comin (ESRF) J. Susini (ESRF) M. Silveira (ESRF-UJF) N. Chevalier (CEA-UJF) S. Huant (UJF-CNRS)

29 IR-SNOM: Test of principle as of Nov MCT Collecting optics? Frequency? x-y-z Focus size? Flux? Spectrometer? Synchrotron Beam conditioning X-Y-Z Grazing angle? Minimizes modification of the current microscope configuration Benefits from existing equipment (microscope + spectrometer)