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Optical Component for Synchrotron Light School on Synchrotron and - - PowerPoint PPT Presentation

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Optical Component for Synchrotron Light School on Synchrotron and Free-Electron-Laser Methods for Multidisciplinary Applications ICTP, 7 th May -18 th May 2018 1 Edoardo Busetto & Luca Rebuffi - MVO Group ICTP, Grignano (TS), 07/05/2018

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

School on Synchrotron and Free-Electron-Laser Methods for Multidisciplinary Applications ICTP, 7th May -18th May 2018

Optical Component for Synchrotron Light

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Optical components for SL: mirrors and monochromators

The most important optical elements for a beamline:

  • mirrors
  • monochromators

mirrors monochromators slits filters sources detectors

low emittance electrons beam produces a high brilliance x-ray photons beam.

“ ...The finite quality and the fundamental limits of the optical components increase the emittance of the beam……. The main aim of the optical design consists on minimizing the inevitable beam degradation…”

Jean Susini “Design parameters for hard x-ray mirrors: the ESRF case” OPTICAL ENGINEERING/February 1995/Vol. 34 2/361

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

If we consider θ as the angle between the incoming radiation and the mirror surface (grazing angle), the x-ray beam will be totally reflected when θ < θc

θ = θc

For x – rays the refraction index is n = 1- δ where 0 < δ < 1, and therefore 0 < n < 1

θ < θc θ > θc

Optical components for SL Mirrors: total reflection

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

1.0 0.8 0.6 0.4 0.2 0.0 Reflectivity 30x10

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26 24 22 20 18 16 14 12 10 8 6 4 2 energy [eV] 0.185 0.180 0.175 0.170 0.150

Curve di riflettività in funzione dell'energia al variare dell'angolo di radenza Materiale del coating : Platino

Angoli di radenza

Grazing angles

Reflectivity as function of the photons energy and the grazing angle in degrees Mirror coating: Platinum

θc = 1.66 λ [A](ρ)1/2[g/cm3]

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Optical components for SL Mirrors: total reflection

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Ellipsoidal surface

Best approximation circle

ρtangential = 2 f / sinϑ ρsagittal = 2 f sinϑ

Tangential focusing Sagittal focusing

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Optical components for SL Mirrors: focusing

an ideal focusing mirror will focus a point source into another point according to the formula 1/q+1/p=1/f

§ Bendin magnet § Extended source (wiggler and undulators)

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A. Laser beam Surface under test Reference Linear array detector

Optical Metrology Lab

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

13 active mirror sections 10 minutes / measurement Total time > 130 minutes voltage stability

  • 400x10
  • 6
  • 200

200 Shape difference (mm) 800 600 400 200 mirror position (mm) Effect of 100V at: 00 01 02 03 04 05 06 07 08 09 10 11 12 13 Shape difference (mm)

  • 300x10-6
  • 200
  • 100

100 Resdual hegiht (mm) 800 600 400 200 mirror position (mm)

  • n 860 mm

all @200V 555 nm P-V 153 nm rms 1st correction 155 nm P-V 34 nm rms 2nd correction 112 nm P-V 25 nm rms

Residual height (mm)

Optical Metrology Lab

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

In last 10 years

  • 200 - 400 mm long flat mirrors:

from ~ 1 µrad to ~ 0.2 µrad rms Ion beam figuring (IBF) now almost normally applied

  • curved mirrors

R=100 m , 100 mm long : 0.45 µrad rms Toroid R=300 m, r = 100 mm, 200mm long : 0.5 µrad rms

  • High quality ellipses

IBF finished, 200mm long: 0.8/1 µrad rms from best ellipse F=900mm / 500mm @ 2.5 / 2 deg Fluid jet polishing ,100 mm long: 0.07 µrad rms from best ellipse F=180 mm / 280mm @ 2.5/ 3 mrad

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Goals for the next 10 years Mirror shape errors Slope errors < 50 nrad rms from best shape : flat and moderate curvature height errors < 0.1 nm rms Improvement of figuring technology Convergence of iterative figuring process Development of fast accurate metrology procedures At synchrotrons At manufacturers

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

K-B system advantages

§

Decoupling vertical and horizontal beam components

§

It is hard to realize thick ellipsoidal mirrors with this demanding demagnification

K-B bendable system advantages

§

Focusing of the 2 sources at different distance with the same couple of mirrors

§

Possibility to change the focal plane position

§

Improvement of the coherent beam wavefront

Optical components for SL Mirrors: figure errors modification

End-stations need hig flux - great demagnification - small focal spot K-B optical system holder

pitch roll M1 M2 M1 M2 FEL focus

Vertical mirror Horizontal mirror

α1,2=2

  • a

b a1,2 = 98754 - 99354 mm b1,2 = 1750 - 1200 mm

K-B active optical system – DiProI

  • L. Raimondi et all. Status of the K-B bendable optics at FERMI@Elettra FEL
  • Proc. Of SPIE Vol.9208 920804-1
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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

§ KAOS PMMA indentation / WFS measurement

Optical microscope 100X

Reconstruction from Hartmann WFS data

https://en.wikipedia.org/wiki/Shack–Hartmann_wavefront_sensor

PMMA ablation imprint Focal spot simulations from metrology

Good agreement between in-house reconstruction, PMMA, simulations (WISE, SRW)

WFS reconstruction at 32 nm: FWHM = 5.7x6.5 µm2

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

§ KAOS PMMA indentation / WFS measurement

Optical microscope 100X

PMMA ablation imprint Focal spot simulations from metrology

Profilometry at best curvature (LTP) Simulations (WISE, SRW)

Good agreement between in-house reconstruction, PMMA, simulations (WISE, SRW)

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

We can sample the dispersed beam with a slit selecting part of it. The spectral resolution will depend on the glass refraction index n, on the slit aperture and on the distance between slits and the optical prism. The glass refraction index depends on the radiation wavelength, the optical prism splits the visible radiation as function of the energy

Dispersion of radiation through the matter: the RIFRACTION

Visible radiation optical PRISM

Optical component for SL: Visible light monochromators

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A. Ordine zero Ordini esterni (-) Ordini interni (+)

d β α

( ) ( )

β α λ sin sin d n − =

Soft X-ray I.R. U.V. Visible Microwave Hard X-ray

The optical surface is machined with particular periodic structures that are origin of interference phenomena with the incoming radiation

GRATINGS

Dispersion of radiation from a periodic structured surface: the surface DIFFRACTION

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Optical component for SL: Soft x-rays monochromators

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Soft X-ray I.R. U.V. Visible Microwave Hard X-ray

Single crystal The Bragg’s law

The radiation penetrates the material and is diffused by the atoms of the structure. The diffused waves interfere. The interference will be constructive if the difference in optical path will be a multiple of the wavelength λ:

Dispersion of radiation from a bulk periodic atomic structure: The bulk DIFFRACTION

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Optical component for SL: Hard x-rays monochromators

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

From the Bragg’s law therefor and the Bragg angle is 90o

2dsinϑ=nλ

sinϑ=1 ⇒ λmax

λmax = 2d

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Optical component for SL: monochromators

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

  • from the derivative of the Bragg’s low an important property of the hard x-ray

monochromators energy resolution Δθ is the convolution of two contributes: Δθ

Δθbeam - angular divergence of the radiation beam in the scattering plane

ωs - the intrinsic angular bandwidth of the crystal monochromator

known as Darwin width

Δλ λ = ΔE E = Δϑ cotg ϑ B

( )

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Optical component for SL: monochromators

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Case with Δθ Δθbeam>> ωs white beam with divergence in the plane of scattering The crystal will diffract all the rays with: θmin ≤ θΒ ≤ θmax monochromator θmin / Emax θmax / Emin

In this case the energy bandwidth is

ΔE ≈ Δθbeam cotg(θB) E Emin Emax

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Optical component for SL: monochromators

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Case with Δθ Δθbeam << ωs white parallel beam in the scattering plane monochromator Vertical collimating mirror parabola

In this case the energy bandwidth will be the crystal Darwin width, function of the Miller indexes: ΔE ≈ ωs cotg(θB) E

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Optical component for SL: monochromators

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Dumond’s diagram

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Optical component for SL: monochromators ωs

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A. Dumond diagram of the first crystal Dumond diagram of the second crystal

Second crystal in non dispersive configuration to achieve a fixed exit beam All rays accepted by the first crystal are accepted also at the second one

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Optical component for SL: Hard x-rays monochromators

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A. Dumond diagram of both crystals Dumond diagram of the first crystal Dumond diagram of the second crystal

Second crystal in dispersive configuration to improve energy resolution Out of axis rays on the first crystal are incident at different angles on the second one.

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Optical component for SL: Hard x-rays monochromators

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

The Darwin curve

INTENSITY OF THE

  • reflectivity or peak reflectivity

REFLECTION

  • integral reflecting power

predicted by the dynamical theory absorption effects

ωs

n

  • rder of the reflection

λ1 wavelength of the fundamental e-M(n) temperature factor V volume of the unit cell ϑB Bragg angle Re radius of the electron e2/mc2 Fhr real part of the structure factor related to the diffracted direction h(h,k,l)

ωs= 2 sin2ϑ B reλ1

2

πV CFhr e−M(n)

angular shift due to the refractive effect

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

the b parameter

defined as : α is the angle between the Bragg plane and the crystal surface

b= sin α-ϑB

⎛ ⎝ ⎜ ⎜ ⎞ ⎠ ⎟ ⎟

sin α+ϑB

⎛ ⎝ ⎜ ⎜ ⎞ ⎠ ⎟ ⎟

ωo = ωs b

the angular acceptance as function of the intrinsic width and the b parameter:

  • T. Matsushita and H. Hashizume X-Ray Monochromators

Handbook on Synchrotron Radiation, Vol. 1

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Bragg reflection width in case of asymmetric cut crystal is defined by:

ωh =ωs b

Sh = So b ωhSh =ωoSo

also for the beams sections combining the two formulas we have the well known Liouville’s theorem the angular acceptance as function

  • f the Bragg reflection width

ωh =bωo

  • T. Matsushita and H. Hashizume X-Ray Monochromators

Handbook on Synchrotron Radiation, Vol. 1

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Τ. Ματσυσηιτα ανδ Η. Ηασηιζυµε Ξ-Ραψ Μονο νοχηρ ηροµατο τορσ Ηανδβοοκ ον Σψνχηροτρον Ραδιατιον, ςολ. 1, εδιτεδ βψ Ε.Ε. Κοχκ Νορτη-Ηολλανδ Πυβλισηινγ Χοµπανψ, 1983

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

  • T. Matsushita and H. Hashizume X-Ray Monochromators

Handbook on Synchrotron Radiation, Vol. 1 27

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

The simplest DCM, the channel-cut.

The chanel-cut DCM is made from a single crystal monolith. Advantages: simple, intrinsically aligned Disadvantages: not fixed height beam output changing the energy

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

1 X

2 + 1

Y

2 = 4

D

2

Pseudo channel-cut Double Crystal Monochromator

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The pseudo chanel-cut DCM is made from two single crystals mounted on to a common rotating table. Advantages: fixed height beam output changing the energy Disadvantages: it needs course and fine regulations for the second crystal

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

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Pseudo channel-cut Double Crystal Monochromator

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

crystal positions: θ 2100 eV 2300 eV 25000 eV =70.3° =59.3° =4.5° θ θ Si(111) II crystal rotation II crystal translation linear slide II crystal movements:

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Independent Double Crystal Monochromator

The first crystal can rotate. The second crystal can rotate and translate. Advantages: fixed height beam

  • utput due to the

mechanical construction along a wide energy range Disadvantages: it needs course and fine regulations for the second crystal

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

10

  • 10

2 3 4 5 6 7 8 910

  • 9

2 3 4 5

ion chamber measured current (A) 20 18 16 14 12 10 8 6 bragg angle (deg)

  • 20
  • 10

10 20 autocollimator pitching parllelism error (arc sec) 18.545Kev 7.950Kev piezo correction (arc sec) 32

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

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Final design 3D view The monochromar equipped with a sagittal bender is operating at the powder diffracion beamline @ Elettra

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

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The XRD1 Double Crystal monochromator @ Elettra it has been designed in Elettra in 1991. It operates since 1994. Recently modified with a LN2 cooling system

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Monochromator optics and thermal load XRD1 Absorbrd power 0.4 kW*

* 1.5 x 0.28 mrad2

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Channels thickness: 300 µm depth: 2 mm

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The two crystal elements before brazing in vacuum oven (first prototype)

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

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Metrology station with X-rays

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

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Metrology station with X-rays

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

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Rasterized crystal point rocking curve @ 1.54 Å Si111 FWHM 10.3 arcsec.

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

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Topography of the internal cooled Si-crystal with channels perpendicular to the scattering plane

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Topography live

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

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Same topography but with channels in the same direction of the scattering plane

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

§ Detector for Hard X-rays § Two large families: single counters integrators

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

§ Single counters : § These systems allow to collect all the electrons produced by the absorption

  • f an x-ray.

§ The mean number of electrons produced during the absorption process is proportional to energy of the single x-ray. § Used in spectroscopy

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

hν e hν x Banda di valenza Banda di conduzione hν x hνe

cristallo scintillatore NaI:Ta fotocatodo stadio moltiplicatore dinodi e

Ta* Ta

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Scintillators

These kind of detectors are the result of the coupling between a doped crystal ( i.e. NaI:Ta) and a photo-multiplier tube

https://en.wikipedia.org/wiki/Scintillation_counter

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

2D Integrators detectors

§ They integrates the charge. Generally losing the direct correlation between electrons produced and energy of the absorbed photon. § The signal local intensity has to be proportional to the dose absorbed in the same region. § Correlation is possible in case of monochromatic beam

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

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Radiographic film (totally analogic) It is still one of the most used detector. Due to the photocemical reaction AgBr –> Ag+ with a density of Ag+ that is proportional to the absorbed radiation. The developer bath reduces Ag+ –> Ag with the tipical gray scale we are used to see .

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

Characteristic curve of the film density versus the time esposure (log/log) Dynamic range Linearity

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

2D integrator detectors (analogic/digital)

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

+ + + + + + Banda di valenza Banda di conduzione hνx hν e Eu

2+

Eu

3+

F F + + + + Banda di valenza Banda di conduzione Eu Eu

3+

+ + + + hνs F F+ hν e F F +

2+

Esposizione ai raggi x fotoluminescenza stimolata

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Imaging Plate… analogical detector with digital readout

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

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2D integrator detectors (totally digital)

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

PILATUS 6M: Specifications No of Modules: 60 Module arrangement: 5 x 12 Detector Size: 431 x 448 mm2 Format: 2527 x 2463 pixels Spatial resolution: 0.172 x 0.172 mm2 Dynamic range/pixel: 20bits Count rate/pixel: <8 Mcps/pixel Readout time: 3.5 ms Frame rate: 12.5 Hz Compressed dimension: ≈ 6M/frame Mechanical positioning: Flat geometry Intermodule gap x: 7 pixels, y: 17 pixels, 8.4% of total area Data storage?……….. Hops! we have a problem!

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ICTP, Grignano (TS), 07/05/2018 Edoardo Busetto & Luca Rebuffi - MVO Group Elettra - Sincrotrone Trieste S.C.p.A.

THANK YOU!

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