I08-SXM beamline @ Diamond; an ambitious project comes true Majid - - PowerPoint PPT Presentation

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I08-SXM beamline @ Diamond; an ambitious project comes true Majid - - PowerPoint PPT Presentation

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I08-SXM beamline @ Diamond; an ambitious project comes true Majid K. Abyaneh, T. Araki, B. Kaulich I08-SXM, Diamond Light Source, UK ILSF, Qazvin - Iran 21 st April, 2015 Villages Phase I Phase II Phase III Macromolecular I02 I04-1 VMXi

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I08-SXM beamline @ Diamond; an ambitious project comes true

Majid K. Abyaneh, T. Araki, B. Kaulich I08-SXM, Diamond Light Source, UK

ILSF, Qazvin - Iran 21st April, 2015

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Villages Phase I Phase II Phase III Macromolecular Crystallography I02 I03 I04 I04-1 I24 VMXi VMXm I23 Spectroscopy I18 (I18) I20 B18 I08 (I08) I14 (I14) I21 Soft Condensed Matter B23 I22 B22(B22) B21 Materials I16 I13 (I13) I19 B16 Engineering & Environment I15 I12 (I12) I11 I15-1 Surfaces & Interfaces I06 (I06) I07 I10 I09 B07 I05 Imaging B24

ILSF, Qazvin - Iran 21st April, 2015

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Diamond X-ray imaging and spectromicroscopy BLs

0.25 2 4 10 20 35 Photon energy range/ keV Beam size at sample 1 mm 1 mm 100 nm 10 nm I08 I13/ I14 I18

? ? Gray zone

B24 B16 I12: 53-150 keV; < 2-3 mm

ILSF, Qazvin - Iran 21st April, 2015

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I08 - Scanning X-ray microscopy

  • Broad photon energy range

(250 – 4200 eV)

  • Highest resolutions down to 20

nm for some imaging modes

  • E/dE = 4000-10000 energy

dependent

  • up to 1010 ph/s in a 20nm spot
  • Various detection modes for

imaging and spectro- microscopy (XANES, LEXRF, electron emission)

  • Versatile specimen

environments

Main specifications

Bridge-DH

ILSF, Qazvin - Iran 21st April, 2015

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I08 - Scanning X-ray microscopy

HU53

ILSF, Qazvin - Iran 21st April, 2015

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I08-SXM BL layout

Control Rooms 1&2/ Specimen Prep Area (±0.5 oC; <40 dB; Office environment) Experiments Cabin (±0.1 oC; <40 dB; Lab environment) Optics Cabin II (±0.5 oC; <45 dB; Optics Cabin I (±0.5 oC; <45 dB) Optics Hutch (±0.5 oC; <50 dB) Airlock Vestibule

Support Lab

ILSF, Qazvin - Iran 21st April, 2015

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I08 – SXM _ Insertion Device

Insertion device 4.5m HU53 due to change of straight section and accessibility of circular polarization to carbon edge

ILSF, Qazvin - Iran 21st April, 2015

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Ni coating stripe Au coating stripe Measurement RMS (Å) PV (Å) RMS (Å) PV (Å) 1 1.46 53 0.98 33 2 0.86 39 0.97 33 3 0.83 40 0.95 36 4 1.05 58 0.88 36 5 0.91 42 0.93 33 Average 1.02 46 0.94 34

Figure 1: Examples of the surface roughness figures (the first two measurements) of the Au stripe. Table 1: The measurement result.

(Removed term: the 2nd order of Zernike polynomial)

Figure 2: Examples of the surface roughness figures (the first two measurements) of the Ni stripe.

Au Ni

I08 – SXM _ Mirrors

ILSF, Qazvin - Iran 21st April, 2015 Sq=Root Mean Square; Sy=Height of Peak to Valley

Manufacturer: Gooch & Housego

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ILSF, Qazvin - Iran 21st April, 2015

I08 – SXM _ Plane Grating Monochromator

Mirror(M2) Grating slots

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Gratings for PGM (DIOS GmbH)

10 mm exit slit; cff=4

I08 – SXM _ Plane Grating Monochromator

ILSF, Qazvin - Iran 21st April, 2015

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I08 – SXM _ Diagnostics

1- Pre-PGM version :water-cooled 2- Post-PGM version :un-cooled

ILSF, Qazvin - Iran 21st April, 2015

  • ut

in

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I08 End station

Static, 4m long granite End station on floating granite Exit slit/ Secondary source Attenuator stage Diagnostics unit

ILSF, Qazvin - Iran 21st April, 2015

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I08 End station

Transmission EMCCD detector system LN2 cryogenic cooling and transfer system X-ray fluorescence detector In-situ visible light microscope Control system for vacuum and cryo transfer

ILSF, Qazvin - Iran 21st April, 2015

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  • Optical components

Zone Plate, OSA, Central Stop,...

  • Sample stage

Stepper motor, Piezo stage

  • Detectors

CCD, SDD, Electron analyser

CCD

Sample stage

SDD

OSA FZP Feedthrough and cabling

ILSF, Qazvin - Iran 21st April, 2015

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I08-SXM End station

Vacuum window ZP stage with scanner XRF detector OSA Laser interferometer Transmission detector system Specimen coarse and fine stage Cryo stage Cold trap

ILSF, Qazvin - Iran 21st April, 2015

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I08 End station - Detectors

Standard detector type to be used ‘simultaneously’ Usage Andor EMCCD Ultra 897 with 512x512px Transmission imaging with simultaneous acquisition

  • f absorption, phase contrast and dark-field, soft X-

ray diffraction, XANES IRD Quad segment photo diode Transmission imaging with simultaneous acquisition

  • f absorption, phase contrast, XANES

Bruker X-Flash 6|100 XRF detector (with a single 100mm2 SDD detector and XIA MCA) Elemental mapping

Other detectors: PMT, Channeltron, in-situ visible light microscope

Conventional set-up

Fibre-optic coupled

ILSF, Qazvin - Iran 21st April, 2015

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I08 End station - Detectors

Low-energy XRF detector system:

ILSF, Qazvin - Iran 21st April, 2015

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I08 End station - Specimen environments

Specimen environment Description Standard dry specimen Kinematic mount with repositioning precision of at least 5 um or less than 10%

  • f the object field

Cryogenic specimen environment LN2 cooled specimen (< -160 oC) with temperature stability < 0.1 oC including transfer system Electrochemical reaction cell (in design phase) Closed chemical reaction cell with electrical biasing, in- and outlet of reactants (liquid and gases) Chemical reactors for new biomaterials (in design phase) Closed chemical microfluidic reaction cell with pH and temperature control Micro heater (under commissioning) Microheater on Si3N4 membrane with temperature sensor (200 oC on day-1; max 500 oC) Magnetic field Specimen with remanent magnetic field, no external magnetic field applicable

ILSF, Qazvin - Iran 21st April, 2015

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Plunge freezing the grids by Leica EM GP

Work flow for sample preparation & transferring in Cryo state

Cryo-stage Not ordered yet

Cryo Microtom

OR

ILSF, Qazvin - Iran 21st April, 2015

Mounting and loading samples under LN2

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Load-Lock

Loading the sample using Leica transferring shuttle

ILSF, Qazvin - Iran 21st April, 2015

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Elements accessible by I08-SXM

250 – 4200 eV X-ray photon energy range

ILSF, Qazvin - Iran 21st April, 2015

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I08-SXM: Primary results

1st order diffraction cone

  • n the CCD camera

15x15 mm 8x6 mm

  • Images acquired with single-element photodiode

ILSF, Qazvin - Iran 21st April, 2015

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I08-SXM: Status update - Imaging Test pattern from zoneplates.com; 720 eV photon energy, 400px x 400px, 1ms dwell/s; Smallest features in the Siemens star are 50 nm 2 mm

ILSF, Qazvin - Iran 21st April, 2015

1 mm Abs DPC

2 mm

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ILSF, Qazvin - Iran 21st April, 2015

I08-SXM: Status update - Imaging nucleous perinuclear region cytosol membrane

  • f soma cell

neuropil Rat cortical neuron cell in brain tissue; 34x36 um, 845 eV Courtesy of C. Poitry-Yamate @ CIBM, EPFL Lausanne, CH 720 eV

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ILSF, Qazvin - Iran 21st April, 2015

N

XRF map & DPC images at RT

Transmission Horizontal Vertical Courtesy of C. Poitry-Yamate @ CIBM, EPFL Lausanne, CH

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C Fe O

2 mm 2 mm

C Fe N cryo-XRF map; Ferihydrate co-prep Geobacter sulfurreducens T < 160 C Courtesy of Prof. J. Lloyd; University of Manchester

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ILSF, Qazvin - Iran 21st April, 2015

NEXAFS spectromicroscopy on Fe nano

  • particles. Courtesy of Neil Telling,

Keele University.

Fe

To explore biomineralised iron deposits in organic materials

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ILSF, Qazvin - Iran 21st April, 2015

Transmission imaging and XRF mapping of particles from a hydrothermal vent orifice in the deep sea; samples provided by Rachel Mills, Southampton University

http://www.pmel.noaa.gov/eoi/ XRF mapping of particles from deep-sea vents

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(D. Wang, RSC, 2013) (D. Wang, Crys Growth Des, 2011) Extracted spectra from 6 images around Sn-edge

STXM images with 30nm resolution @510 eV

480 eV 495 eV 510 eV

200 nm

A B

1 um

ILSF, Qazvin - Iran 21st April, 2015

CNTs on the ITO surface

  • A. Goldoni et. al., Elettra (2015)
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I08 - Scanning X-ray microscopy

  • 250 - 2000 eV photon energy

range

  • Resolutions far below 10 nm,

resolution-limited only by the wavelength

  • Achromatic design
  • Potential for absorption and

phase spectroscopies on nanoscopic scales

  • Novel depth-profiling

techniques not possible with conventional SXM techniques

Side branch for soft X-ray diffraction imaging (Ptychography)

Ptychographic reconstruction

  • f amplitude and phase

images of a mouse fibroblast cell doped with cobaltferrite ENPs (pilot experiment performed at TwinMic, Elettra) Collaboration with Sheffield University and University College London

ILSF, Qazvin - Iran 21st April, 2015

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Visit us at: http://www.diamond.ac.uk/Beamlines/Spectroscopy/I08.html Follow us on: https://www.facebook.com/DiamondLightSource https://twitter.com/DiamondLightSou/ I08-SXM local Contacts:

  • Dr. Burkhard Kaulich: Principal Beamline Scientist

burkhard.kaulich@diamond.ac.uk

  • Dr. Majid Abyaneh: Senior Support Scientist

majid.abyaneh@diamond.ac.uk

Thank You

ILSF, Qazvin - Iran 21st April, 2015