Multilayers in synchrotron optics Ch. Morawe, J-Ch. Peffen, K. - - PowerPoint PPT Presentation

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Multilayers in synchrotron optics Ch. Morawe, J-Ch. Peffen, K. - - PowerPoint PPT Presentation

Multilayers in synchrotron optics Ch. Morawe, J-Ch. Peffen, K. Friedrich, M. Osterhoff Outline Mirrors and multilayers Design and fabrication Performance and applications Summary and perspectives Ch. Morawe - ESRF Friday


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  • Ch. Morawe - ESRF Friday Seminar 21.05.10

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Multilayers in synchrotron optics

  • Ch. Morawe, J-Ch. Peffen, K. Friedrich, M. Osterhoff

Outline

  • Mirrors and multilayers
  • Design and fabrication
  • Performance and applications
  • Summary and perspectives
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  • Beamline Control Unit (software development)
  • Mechanical Engineering and Modelling (bender development)
  • Data Analysis Unit (theory and simulation)
  • Experiments Division (various beamlines)
  • X-ray Optics Group (metrology)
  • Collaborations with APS, NSLSII, Spring-8, Osaka University …

Acknowledgements

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Mirrors and multilayers

Basic geometry

F S p q

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Mirrors and multilayers

n2 < n1

Interaction of X rays with matter

Optical index Snell’s law Critical angle of total reflection In vacuum:  Total reflection x-ray mirrors (TRM) But: @ E = 10 keV:  Very long mirrors at high energies!

1 1 n i      

1 2 2 1

cos cos n n   

2 1

cos

C

n n   2

e C

E      

5 0.3

C

mrad    

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Mirrors and multilayers

Total reflection mirror

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Mirrors and multilayers

Single surface reflection  Multiple reflections  Multilayer

Recursive calculation of Fresnel coefficients and propagation

  • Parratt

formalism (widely used in x-ray optics) Principle

  • Start at semi-infinite substrate surface (no reflection from back side)
  • Recursive construction of amplitudes and phases from layer to layer

fn-1,n : Fresnel coefficients En : Electric field at centre of layer n tn : Thickness of layer n

2 1 ,

r R 

n R n n n n

E E a r

2 1 ,

   

2 2 2

cos n n t i n

n n

e a

  

           

     

1

, 1 1 , , 1 1 , 4 1 , 1 n n n n n n n n n n n

f r f r a r

Substrate

L.G. Parratt, Phys. Rev. 95, 359 (1954)

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Mirrors and multilayers

Numerical simulation

Main features

  • Bragg peaks and fringes due to interference
  • Positions depend on E and Λ
  • Intensities depend on ∆ρ, N, σ…

Corrected Bragg equation

For θ >> θC 

B A

  • sin

 sin 2      m  

2 2 1 2 2

cos 2 n n m      

ML reflectivity spectra

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Mirrors and multilayers

X-ray reflectivity measurements and simulations

10-6 10

  • 5

10

  • 4

10-3 10

  • 2

10-1 100 0° 1° 2° 3° 4° 5° 6° Reflectivity 

[Ir/Al2O3]10

Simulation of x-ray reflectivity

Vertical density profile

4 8 12 16 20 24 5 10 15 20 25 Mass density [g/cm

3]

Sample depth [nm]

[Ir/Al2O3]10 (Al

2 

(Si) (Ir)

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Mirrors and multilayers

Transmission electron microscopy (TEM)

  • Fabrication errors
  • Roughness evolution
  • Crystallinity
  • Interface diffusion

Complementary to x-ray measurements !

  • R. Scholz, MPI Halle, Germany

[W/B4 C]50

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Mirrors and multilayers

decreasing d-spacing  increasing Bragg angle

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Mirrors and multilayers

Reflecting multilayer

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Design and fabrication

Materials choice – Basic rules

1. Select low-Z spacer material with lowest absorption (βspacer ) 2. Select high-Z absorber material with highest reflectivity with spacer (δabs – δspacer ) 3. In case of multiple choices select high-Z material with lowest absorption (βabs ) 4. Make sure that both materials can form stable and sharp interfaces (lower d-spacing limit)

Computational search algorithms

  • Soft X-rays: A.E. Rosenbluth

(1988)

  • Hard X-rays: K. Vestli

(1995)

Areas of application

  • EUV lithography (E = 94 eV)
  • “Water window”

(E = 280…550 eV)

  • “Hard”

X rays (E = 1…100 keV)

  • K. Vestli, E. Ziegler, Rev.Sci.Instr. 67, 3356 (1996)
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Design and fabrication

Filling factor (Gamma ratio)

  • Γ

= tabs /Λ

  • Harmonics suppression
  • Reflectivity enhancement

tabs tspace

1st 2nd 3rd

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Design and fabrication

Energy resolution of multilayers – Experimental results

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Design and fabrication

Reflective x-ray optics - Integrated reflectivity versus energy resolution

Integrated reflectivity 

R(peak) = 100% Single Crystals Traditional ML's High-resolution ML's Depth-graded ML's

Be

110

Si

111

Ge

111

(Mirrors/Filters) forbidden area E = 8 keV 10-6 10-5 10-4 10-3 10-2 10-1 100 10-6 10-5 10-4 10-3 10-2 10-1 100

ESRF MLs

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Design and fabrication

Reflecting multilayer strong lateral thickness gradient

x z

weak normal thickness gradient

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Design and fabrication

Lateral d-spacing gradient depending on surface curvature and beam divergence Shape Angle  d-spacing including refraction correction (modified Bragg equation) Parabola Ellipse

sin  p 2 f sin  b pq sin  s f

Flat Geometry

q p b 

f  s f p/2 

 

2 2

cos 2     n m

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Differential deposition      

L m s m s m L

dx t x R f x x v x

 

 

Flux Speed Thickness

Substrate Mask Source

Design and fabrication

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Design and fabrication

Uniform coating area up to 1000mm x 150mm Loading bay Load lock Deposition zone Escape area Escape area

ESRF ML deposition facility Major upgrade in 2008

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Design and fabrication

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Design and fabrication

Experimental results Specular reflectivity Thickness profile

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Design and fabrication

Fabrication history

  • More than 100 devices delivered since 1998
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Performance and applications

Multilayer high flux monochromators

  • Two bounce optics
  • 100x larger bandwidth compared with Si(111)
  • Harmonics suppression due to refraction and filling factor
  • Radiation and heat load issues !
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Performance and applications

Total-reflection X-Ray Fluorescence (TXRF) for trace analysis (MEDEA)

  • Undulator source: P > 100 W @ E = 1…20 keV
  • Vertical double bounce ML monochromator
  • Two ML stripes: [Ru/B4

C]40 and [Ir/Al2 O3 ]100

  • Flux gain 100…1000 compared with Si(111)
  • Metal contamination on Si wafers
  • Detection limit < 1010

Atoms/cm2 (Ni)

2nd crystal (uncooled) Picomotor Copper plate Alignement system 1st crystal (cooled)

Beam in

  • G. Apostolo
  • F. Comin
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Performance and applications

Old deposition system

[W/B4 C]40 : Λ = 4.0 nm Strong thickness decay (4% PV)

New deposition system

[W/B4 C]120 : Λ = 2.0 nm Residual d-spacing error <1% PV

Double [W/B4 C] ML monochromator for ID17 (Bio-Medical imaging)

  • Double bounce ML monochromator

100mm long and 150mm wide (each)

  • 2 uniform and identical ML coatings, both in 1 run
  • D-spacing mapping via x-ray reflectivity
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Performance and applications

Double ML monochromator for ID09B (Pump and probe)

  • Double bounce ML monochromator

after heat load chopper

  • Two ML stripes [Ru/B4

C]40 and [Ir/Al2 O3 ]100 Pink beam Asymmetric spectrum @ 18 keV

0.3 s exposure

ML beam Symmetric spectrum with dE/E = 1.6% @ 25 keV)

3 s exposure Courtesy M. Wulff

Si powder

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Performance and applications

White beam exposure (K. Friedrich)

  • Cryogenic test bench and undulator

beam

  • Heat load versus photon irradiation
  • X-ray reflectivity  ML structure, diffusion
  • Interferometry

 Surface figure

  • Thermal expansion and stress
  • Simulation by finite element analysis
  • Improved coatings
  • Engineering solutions

X-rays ML LN tank window Interferometer

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Performance and applications

Kirkpatrick-Baez (KB) focusing devices

  • Separate vertical and horizontal focusing (non-circular source)
  • Technologically easier than single reflection ellipsoid
  • Metal or graded ML coatings
  • P. Kirkpatrick, A.V. Baez, J. Opt. Soc. Am. 38, 766 (1948)

Albert V. Baez was the father of Joan Baez !

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Static KB mirrors

  • Ultimate accuracy with static figuring, but no energy tunability

with MLs

Performance and applications

Spring-8/Osaka University (Japan): Deterministic polishing

  • S. Matsuyama et al, Rev. Sci. Instr. 77, 093107 (2006)
  • C. Liu et al, Ref. Sci. Instr. 76, 113701 (2005)

APS-ANL (USA): Profile coatings

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Dynamically bent KB mirrors at ESRF

  • Lower ultimate accuracy, but more flexibility in energy and shape

Performance and applications

Different configurations:

  • Single bender
  • KB 112-76
  • KB 170-96
  • KB 170-170
  • KB 170-300
  • KB 300-300

96 mm 170 mm 300 mm

* O.Hignette et al., AIP Conf Proc. 879, 792 (2007) ID23 5 x 7 µm ID27 2 x 4 µm ID13 0.3 x 0.4 µm ID22NI 76 x 84 nm ID19 45 nm line focus*

Spot size:

ESRF BLs since 1998: 65 benders installed 43 ML coatings

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Performance and applications

ID22NI:

High β @ 60 m, slit source, E = 17 keV 76x84 nm2: 109ph/s @ 200mA 150x100 nm2: 1012ph/s @ 200mA

ID19:

Low β @ 150 m, E = 15…24 keV 86x83 nm2: 2·1011ph/s @ 80mA

3·105 ph/s/mA/nm2

  • P. Cloetens, O. Hignette, ESRF
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Performance and applications

[W/B4 C] MLs (KB system Nano-Imaging BL ID22NI)

  • Photon energy E = 17.0 keV, Source at 36(H)/63(V) m / BL upgrade  157(H)/185(V) m
  • Central grazing angle 

= 8 mrad = 0.46° Focusing geometry ML structure  [nm] / L [mm] q [mm] Spot [nm] Vertical [W/B4 C]25 4.9 38% 112 180 60 Horizontal [W/B4 C]25 4.9 56% 76 83 50

Courtesy

  • R. Baker
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Performance and applications

Wave optical simulation of total reflection mirrors (M. Osterhoff)

  • Fresnel reflection + propagation
  • Finite source size + measured surface figure
  • Upgrade to curved MLs

in progress…

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Performance and applications

Limits of x-ray focusing

Diffraction Source size Increased aperture with graded MLs Approximation Present record at Spring-8/Osaka University

0.44

FWHM

D NA   S p q D  

2 1

0.88 5 1 1

FWHM

D nm     

KB focusing history

  • H. Mimura et al, Nature Physics, doi:10.1038/nphys1457 (2009).

?

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  • MLs attractive alternative to mirrors and crystals
  • Solution of choice for high flux and medium resolution applications
  • ML based focusing setups < 100 nm operational, < 10 nm demonstrated
  • ESRF ML activity for more than 15 years
  • More than 100 devices delivered to ESRF beamlines
  • Crucial element in the ESRF Upgrade Programme
  • Further development to improve stability (white beam)
  • Coherence preservation studies
  • Wave optical simulations

Summary and perspectives

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Thank you for your attention