I08-SXM Diamond; an ambitious project comes true. Majid K. Abyaneh, T. Araki, B. Kaulich I08-SXM, Diamond Light Source, UK

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1 I08-SXM Diamond; an ambitious project comes true Majid K. Abyaneh, T. Araki, B. Kaulich I08-SXM, Diamond Light Source, UK

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

3 Photon energy range/ kev Diamond X-ray imaging and spectromicroscopy BLs 35 B16 I12: kev; < 2-3 mm Gray zone I18 B24 I13/ I14 I08?? 1 mm 1 mm 100 nm 10 nm Beam size at sample

4 I08 - Scanning X-ray microscopy Bridge-DH Main specifications Broad photon energy range ( ev) Highest resolutions down to 20 nm for some imaging modes E/dE = energy dependent up to ph/s in a 20nm spot Various detection modes for imaging and spectromicroscopy (XANES, LEXRF, electron emission) Versatile specimen environments

5 I08 - Scanning X-ray microscopy HU53

6 I08-SXM BL layout Optics Cabin II (±0.5 o C; <45 db; Control Rooms 1&2/ Specimen Prep Area (±0.5 o C; <40 db; Office environment) Optics Cabin I (±0.5 o C; <45 db) Optics Hutch (±0.5 o C; <50 db) Airlock Vestibule Experiments Cabin (±0.1 o C; <40 db; Lab environment) Support Lab

7 I08 SXM _ Insertion Device Insertion device 4.5m HU53 due to change of straight section and accessibility of circular polarization to carbon edge

8 Ni coating stripe I08 SXM _ Mirrors Table 1: The measurement result. (Removed term: the 2 nd order of Zernike polynomial) Au coating stripe Measurement RMS (Å) PV (Å) RMS (Å) PV (Å) Average Manufacturer: Gooch & Housego Au Ni Sq=Root Mean Square; Sy=Height of Peak to Valley Figure 1: Examples of the surface roughness figures (the first two measurements) of the Au stripe. Figure 2: Examples of the surface roughness figures (the first two measurements) of the Ni stripe.

9 I08 SXM _ Plane Grating Monochromator Grating slots Mirror(M2)

10 I08 SXM _ Plane Grating Monochromator Gratings for PGM (DIOS GmbH) 10 mm exit slit; c ff =4

11 I08 SXM _ Diagnostics 1- Pre-PGM version :water-cooled 2- Post-PGM version :un-cooled out in

12 I08 End station Diagnostics unit Attenuator stage Exit slit/ Secondary source End station on floating granite Static, 4m long granite

13 I08 End station Transmission EMCCD detector system In-situ visible light microscope LN2 cryogenic cooling and transfer system Control system for vacuum and cryo transfer X-ray fluorescence detector

14 Optical components Zone Plate, OSA, Central Stop,... Sample stage Stepper motor, Piezo stage Detectors CCD, SDD, Electron analyser Feedthrough and cabling FZP OSA CCD Sample stage SDD

15 I08-SXM End station Transmission detector system Specimen coarse and fine stage OSA Laser interferometer ZP stage with scanner Vacuum window Cryo stage Cold trap XRF detector

16 I08 End station - Detectors Standard detector type to be used simultaneously Andor EMCCD Ultra 897 with 512x512px IRD Quad segment photo diode Usage Transmission imaging with simultaneous acquisition of absorption, phase contrast and dark-field, soft X- ray diffraction, XANES Transmission imaging with simultaneous acquisition of absorption, phase contrast, XANES Bruker X-Flash 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

17 I08 End station - Detectors Low-energy XRF detector system:

18 I08 End station - Specimen environments Specimen environment Standard dry specimen Cryogenic specimen environment Electrochemical reaction cell (in design phase) Chemical reactors for new biomaterials (in design phase) Micro heater (under commissioning) Magnetic field Description Kinematic mount with repositioning precision of at least 5 um or less than 10% of the object field LN2 cooled specimen (< -160 o C) with temperature stability < 0.1 o C including transfer system Closed chemical reaction cell with electrical biasing, in- and outlet of reactants (liquid and gases) Closed chemical microfluidic reaction cell with ph and temperature control Microheater on Si3N4 membrane with temperature sensor (200 o C on day-1; max 500 o C) Specimen with remanent magnetic field, no external magnetic field applicable

19 Work flow for sample preparation & transferring in Cryo state Cryo Microtom Plunge freezing the grids by Leica EM GP OR Cryo-stage Not ordered yet Mounting and loading samples under LN2

20 Loading the sample using Leica transferring shuttle Load-Lock

21 Elements accessible by I08-SXM ev X-ray photon energy range

22 I08-SXM: Primary results Images acquired with single-element photodiode 1 st order diffraction cone on the CCD camera 15x15 mm 8x6 mm

23 I08-SXM: Status update - Imaging 1 mm Abs DPC 2 mm 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

24 I08-SXM: Status update - Imaging nucleous cytosol membrane of soma cell perinuclear region neuropil 720 ev 34x36 um, 845 ev Rat cortical neuron cell in brain tissue; Courtesy of C. CIBM, EPFL Lausanne, CH

25 XRF map & DPC images at RT Transmission N Horizontal Vertical Courtesy of C. CIBM, EPFL Lausanne, CH

26 cryo-xrf map; Ferihydrate co-prep Geobacter sulfurreducens T < 160 C C Fe N 2 mm Courtesy of Prof. J. Lloyd; University of Manchester C Fe O 2 mm

27 To explore biomineralised iron deposits in organic materials Fe NEXAFS spectromicroscopy on Fe nano particles. Courtesy of Neil Telling, Keele University.

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

29 CNTs on the ITO surface A. Goldoni et. al., Elettra (2015) Extracted spectra from 6 images around Sn-edge STXM images with 30nm ev 1 um 480 ev B A 495 ev 510 ev (D. Wang, RSC, 2013) 200 nm (D. Wang, Crys Growth Des, 2011)

30 I08 - Scanning X-ray microscopy Side branch for soft X-ray diffraction imaging (Ptychography) ev photon energy range Resolutions far below 10 nm, resolution-limited only by the wavelength Achromatic design Ptychographic reconstruction of amplitude and phase images of a mouse fibroblast cell doped with cobaltferrite ENPs (pilot experiment performed at TwinMic, Elettra) Potential for absorption and phase spectroscopies on nanoscopic scales Novel depth-profiling techniques not possible with conventional SXM techniques Collaboration with Sheffield University and University College London

31 Thank You Visit us at: Follow us on: I08-SXM local Contacts: Dr. Burkhard Kaulich: Principal Beamline Scientist Dr. Majid Abyaneh: Senior Support Scientist