First test experiments with FMB- Oxford direct drive DCM at the Sirius beamline of Synchrotron SOLEIL Ciatto G., Moreno T., Aubert N., Feret P., Fontaine P. Synchrotron SOLEIL, L'Orme des Merisiers, Saint-Aubin, BP 48, F-91192 Gif sur Yvette CEDEX Email: gianluca.ciatto@synchrotron-soleil.fr
Outline The Sirius beamline at SOLEIL: experimental requirements and optical path chosen The FMB-Oxford DCM: direct drive vs. worm wheel DCM geometry and specifications, offline tests Performances at fixed energy (XRD test experiments) Performances in energy scan (XAS test experiments) Issues and correction strategies
PSD PSD The Sirius beamline at SOLEIL: experimental requirements Large angle scattering Fluorescence (XAS) θ in ~2mrad c GIXD Small angle scattering Reflectivity GISAXS Energy range: 1.4 12 kev tender x-ray variable polarisation Goal: to combine different scattering and spectroscopy techniques at grazing incidence for surface/interface studies GIXD, GISAXS, FLY-XAS, DAFS, Reflectivity, XRMS
The MOON project (ANR) In situ / in operando experiments Monitoring the nucleation process and the early stages of MOCVD/ALD growth of ZnO via X-ray techniques We need fast scanning to follow kinetics!
The Sirius beamline at SOLEIL: technical solutions/selected optics Mirror M4 - Flat, face down: deflection Mirror M1 spherical : MGM flat : DCM Mirror M3 Harmonic rejection Mechanical bender 2 coating (Pt, C) Horizontal focalization (5 µm) Mirror M2 Mechanical bender 2 coatings (Pt, C) Vertical focalization (5 µm) Multilayer Grating Monochromator Undulator Double crystal (Apple II - Monochromator, HU36) Two tracks (Si 111, InSb 111). 18.5 m from source Energy range: 1.4 12 KeV Flux: ~ 1 13 photons/s Beam size:.5 x.5 mm 2 2 (3) end-stations
The FMB-Oxford DCM: worm-wheel vs. direct drive worm - wheel direct drive (torque) Sirius DCM uses a synchronous brushless motor (ETEL) with 44 poles (22 pairs) backlash-free and dynamic response Renishaw encoder + interpolator = 144x1 6 counts/revolution
The FMB-Oxford DCM: worm-wheel vs. direct drive Parameter Worm Wheel Direct Drive Resolution <.4 arc seconds (.18 µrad) <.2 arc seconds (.9 µrad) Repeatability <.15 (.7 µrad) over 35 <.2 (1 µrad) over 9 <.1 (.45 µrad) over 35 <.15 (.7 µrad) over 9 Velocity Range. 1 /sec - 1 /sec. 1 /sec - 4 /sec Velocity Accuracy* 1.5% (2 at.5 /s).1% (2.5 at 1 /s) Settling Time* 15ms from.5 /s 5ms from 1 /s Direct drive enables Slightly better repeatability Superior dynamic performances Very small increments without any backlash With 4 /s at 1 kev we can cover ~ 7 ev in.2 s kinetics monitoring
DCM geometry and specifications Bragg Two crystal pairs: Si (111) and InSb (111) selected by translation of the whole vessel Perpendicular translation of 2 nd crystal for fixed exit (xtal2perp) Beam walks on the second crystals (longer) Very large Bragg angle range (3 to 85 ) and xtal2perp (9-73mm crystal separation) to allow access to 2 KeV with Si (111)
Encoder reading (cts) Encoder reading (cts) Measurements with DCM internal encoder Measurements with Zygo ZMI-2 laser interferometer DCM typical offline tests at the factory Bragg angle increased in steps of 1 cts every 2s Encoder resolution 4 cts per 1 deg 5 readings every 1 ms averaged at each angle, repeated 1 times with step = 2 deg Repeatability < 1 cts i.e.,436 μrad Time (s) Stability during rep. test measured by encoder Stability over 2 s =,48 μrad Time (s)
Intensity ( position (mm Performances at fixed energy (on line) 4.89 vertical position horizontal position Intensity.8 4.88.6 4.87.4 4.86 4.85 4.84 4.83 4.82 5 1 1 4 1.5 1 4 2 1 4 2.5 1 4 3 1 4 3.5 1 4 4 1 4 time (s) 4.88 4.875 4.87 4.865 4.86 4.855 4.85 4.845 4.84 2.25 1 4 2.325 1 4 2.4 1 4 2.475 1 4 Vertical beam movement of 24 µm in ~12 hours Intensity.2 -.2 -.4 -.6 Horizontal beam movement of 18 µm in ~12 hours Intensity variation <.4 % in ~12 hours Beam intensity and position monitored with 4Q sccvd diamond [thickness =5µm, φ= 4mm, gap=5µm]. 27 m from source. K. Desjardins et al., Journal of Physics Conferences Series 425, 2124, (213) No stabilisation feedback
horizontal position (mm) horizontal position (mm) vertical position (mm) vertical position (mm) Performances at fixed energy.8 xbpm after DCM -.54 -.3 xbpm after DCM.42.75 xbpm before DCM -.545 -.35 xbpm before DCM.415.7 -.55 -.4.41.65 -.555 -.45.45.6 -.56 -.5.4.55 -.565 -.55.395.5 5 1 1 4 1.5 1 4 2 1 4 2.5 1 4 3 1 4 3.5 1 4 4 1 4 time (s) -.57 -.6 1 1 4 2 1 4 3 1 4 4 1 4 time (s) Horizontal and vertical beam movements not due to the source, they origin from the DCM.39
xbpm intensity (microa) machine current (ma) Performances at fixed energy 4.89 4.88 current on xbpm 2 machine current 436 435 4.87 434 4.86 433 4.85 432 4.84 431 4.83 43 4.82 5 1 1 4 1.5 1 4 2 1 4 2.5 1 4 3 1 4 3.5 1 4 4 1 4 time (s) Intensity variations read by XBPM2 not related to oscillation in machine current 429
Second crystal pitch (deg) Second crystal Z (mm) Performances at fixed energy vertical beam movement-xbpm 2 (mm) vertical beam movement-xbpm 2 (mm) Bragg angle (deg) Second crystal roll (deg) horizontal beam movement-xbpm 2 (mm) vertical beam movement-xbpm 2 (mm).23436.23435.23434.23433.23432 2nd crystal pitch beam vertical movement (XBPM 2) -.35 -.4 -.45 -.5 -.55.23431 -.6 1 1 4 2 1 4 3 1 4 4 1 4 5 1 4 9.892 time (s) second crystal perp (mm) beam vertical movement (XBPM 2) -.35 V 2 nd crystal pitch, roll and perp (along with Bragg) do not change within repeatability specifications V 14.31243 14.31243 14.31243 14.31242 14.31241 14.31241 14.3124 14.3124 bragg angle beam vertical movement (XBPM 2) 14.31239 5 1 1 4 1.5 1 4 2 1 4 2.5 1 4 3 1 4 3.5 1 4 4 1 4 -.73274 time (s) -.35 -.4 -.45 -.5 -.55 -.6 2nd crystal roll horizontal beam movement (XBPM 2).8 9.8918 9.8916 9.8914 9.8912 9.891 5 1 1 4 1.5 1 4 2 1 4 2.5 1 4 3 1 4 3.5 1 4 4 1 4 time (s) -.4 -.45 -.5 -.55 -.6 V But this can still give a movements of 13 microns for pitch and roll!! H -.73275 -.73276 -.73277 -.73278 -.73279 -.7328 5 1 1 4 1.5 1 4 2 1 4 2.5 1 4 3 1 4 3.5 1 4 4 1 4 time (s).75.7.65.6.55
Performances at fixed energy/issues Stability issues may be due to the fact that we do not use water cooling OUT IN Water connectors too close to LN one: freezing when water supply fails! Home-made solution: it does not work yet. Improving it or chiller solution.
horizontal position (mm) vertical position (mm) Performances at fixed energy - XRD XRD test on low-density zincblende InP nanowires on Si substrate.73 -.4 horizontal position (XBPM 2) (2) reflection of zb InP NWs.72.71.7 vertical position (XBPM 2) -.41 -.42 -.43 (2) reflection of zb InP NWs.69 -.44 (L).68 2 4 6 8 1 12 time (s) -.45 We can obtain satisfying XRD data (even at GI) since the flux is high and beam movements are small over the integration time (<1 μm in 1 s) Grazing incidence
Performances in energy scan monitor intensity (microa) xanes (arb. units) Scans are performed by moving simultaneously monochromator Bragg angle and undulator gap 2 7 E Rs2 5. -.7134 6. -.7121 7. -.7333 8. -.7335 9. -.7337 1. -.73 11. -.73 Tables used for 2 nd crystal pitch, roll and perp calibration during scan 6.5 6 5.5 5 4.5 monitor intensity (xbpm2) xanes 4 7.5 7.6 7.7 7.8 7.9 8 8.1 energy (ev) 15 1 5 No piezo used, no feedback to stabilise beam position/intensity Step observed in XANES, not in monitor, spoils the spectrum
Beam position, XBPM 2 (mm) Performances in energy scan XANES Beam horizontal position (mm) 2nd crystal roll (deg).2 vertical position (xbpm2) horizontal position (xbpm 2) xanes 15.2 horizontal position (xbpm 2) 2nd crystal roll -.7332.15.19 -.7333.1 1.18 -.7334.5.17 -.7335 5.16 -.7336 -.5.15 -.7337 -.1 7.5 7.6 7.7 7.8 7.9 8 8.1 Energy (ev) Step corresponds to beam horizontal movement of 4 microns.14 -.7338 7.5 7.6 7.7 7.8 7.9 8 8.1 Energy (ev) Beam horizontal movement is related to change in 2 nd crystal roll (5*1-4 deg) Problem with roll resolution!! (due to Tango, not to Mono)
Horizontal position, XBPM 2 (mm) Performances in energy scan 2nd crystal roll (deg) Vertical position, XBPM 2 (mm) 2nd crystal pitch (deg).3 -.73245.4.25 -.73241.3 -.732415.2.2 -.73242 2nd crystal pitch vertical position.234.23399.23398.23397.23396.15 2nd crystal roll -.732425.1.23395.1 horizontal position -.73243.23394.23393.5 -.732435 7.6 7.8 8 8.2 8.4 8.6 8.8 energy (ev) -.1.23392 7.6 7.8 8 8.2 8.4 8.6 8.8 energy (ev) Second roll fixed to average of optimized values in energy range of interest. Pitch and roll do not vary more than repeatability now, but there are important beam movements during the scan.
Beam position, XBPM-2 (mm) Performances in energy scan Monitor intensity (microa) Beam position (mm) Beam position (mm).4.3 vertical position horizontal position monitor intensity 7 6.4.2.4.2.2 5 4 -.2 XBPM 2 (after mono) - vertical position XBPM 2 (after mono) - horizontal position -.2.1 3 -.4 XBPM (before mono) - vertical position XBPM (before mono) - horizontal position -.4 2 -.6 -.6 -.1 1 7.6 7.8 8 8.2 8.4 8.6 8.8 energy (ev) -.8 7.6 7.8 8 8.2 8.4 8.6 8.8 energy (ev) -.8 Beam movements after DCM larger than source movements, even if a contribution from the source is possible, especially in horizontal. Main contribution comes from the DCM.
Performances in energy scan Absorption coefficient (arb. units) Magnitude of Fourier Transform (Å -3 ) k 2 (k) Zn.95 Co.5 O thin film, Co K-edge exafs 2 2 1 1.5-1 -2 1 5 1 15 k (Å -1 ) Spectra at 1s/point max at the present.5 76 78 8 82 84 Energy (ev) 2 4 6 8 1 R (Å) No more steps and good exafs spectra of dilute elements in nanostructures possible at Sirius fixing the crystal 2 roll, even without feedback.
Absorption coefficient (arb. units) k 2 (Å -3 ) Performances in energy scan exafs 1.2.8 Incidence angle =.29 deg (close to critical one) 1.4 Incidence angle =.29 deg (close to critical one) -.4.5 -.8 Grazing incidence 76 78 8 82 84 Energy (ev) -1.2 5 1 15 k (Å -1 ) Also grazing incidence EXAFS feasible by placing a 5-1 micron slit before the sample to define beam spot (samples 5x5 mm)
XANES Monitor intensity Vertical movement (XBPM2) (mm) 2nd crystal Z (mm) Performances in energy scan/issues 6.5 6 5.5 5 4.5 XANES XBPM2 intensity 16 14 12 1 8 6 4.15.1.5 -.5 vertical position (xbpm 2) 2nd crystal Z translation 24 22 2 18 16 14 4 2.2 2.3 2.4 2.5 2.6 2.7 2.8 2.9 3 Energy (ev) 2 -.1 12 2.2 2.3 2.4 2.5 2.6 2.7 2.8 2.9 3 Energy (ev) Problems in beam intensity stabilisation during scans at low energy (< 3 kev) due to large variation of 2 nd crystal perp. translation many points needed in table. Solutions: use of piezo on 2 nd crystal perp/feedback? InSb instead of Si at E < 3?
Issues and correction strategies Solving problem with 2 nd crystal roll minimum step (Tango configuration): done! New test to re-introduce water cooling for long time stabilization Improving stability in beam position using one or two of the piezo on pitch/roll/perp (depending on experiment) along with the I-2 two-channel digital electrometer with analog output for servo control (Successfully tested at other beamlines in SOLEIL!) Increase of velocity in scans to fully exploit the DCM dynamics thanks to continuous energy scan/fly scan