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X-ray optics ray optics X-ray optics ray optics Crystal optics Crystal optics Crystal optics Crystal optics Jürgen Härtwig Jürgen Härtwig Jürgen Härtwig ESRF X-ray Optics Group, Crystal Laboratory Jürgen Härtwig ESRF X-ray Optics Group, Crystal Laboratory X X - - ray Optics Group ray Optics Group O O G G X X X X - - ray Optics Group ray Optics Group O O G G X X O O G G X X ESRF

XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

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Page 1: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

XX--ray opticsray opticsXX--ray opticsray opticsCrystal opticsCrystal opticsCrystal opticsCrystal optics

Jürgen HärtwigJürgen HärtwigJürgen Härtwig

ESRF X-ray Optics Group, Crystal Laboratory

Jürgen Härtwig

ESRF X-ray Optics Group, Crystal Laboratory

XX--ray Optics Groupray Optics Group

OOGGXXXX--ray Optics Groupray Optics Group

OOGGXXOOGGXXESRF

Page 2: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

What was already presented (among others)?

Physics of the electron beam source (Boaz Nash)

Ph i f X di ti d ti d t t (M l Physics of X-ray radiation production and transport (Manuel Sánchez del Río)

Multilayers in synchrotron optics (Christian Morawe)

Energy resolving detectors for X-ray spectroscopy (John Morse)

So we continue today with the X-ray opticsSo we continue today with the X ray optics

Page 3: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

OutlineOutline

1. Introduction

2. Monochromators

3 S ti f t i l fl ti3. Some properties of asymmetrical reflections

4. Shortly about high energy resolution

5. Crystal quality and how to measure it

(6 Plane or divergent monochromatic or (6. Plane or divergent, monochromatic or polychromatic waves in our experiments?)

Page 4: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

1. Introduction1. Introduction1. Introduction1. IntroductionSome questions I plan to discuss and maybe to answer:Which kind of monochromators are used? How may I change the energy

l ti b di b di i ?resolution, beam divergence, beam dimension?

May the Bragg diffraction geometry have an influence on the coherence?

R l f i d l i I fl t l Role of source size and angular source size. Influence on transversal coherence, resolution etc. ?

Are “Imaging quality” “focusing properties” “coherence preservation” Are Imaging quality , focusing properties , coherence preservation related?

What is a “highly perfect” crystal? What are the lowest strains that we can measure?

Is there a “highly parallel (monochromatic)” beam? Is there a “nanometric parallel” beam?parallel beam?

We need to define what a “plane” or a “monochromatic” wave could be in the real experimental life. How may we approximate them?p y pp

etc.

Page 5: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Optical system / experimental set-up:Optical system / experimental set up:Source optical elements sample optical elements detector

The task of the optics:To transform the beam to obtain the best matching with the o transform the beam to obta n the best match ng w th the experiment; not loosing the good properties of the beam after its creation.

It acts on:- shapeshape- wavelength/energy- divergence- polarisation- coherence

Page 6: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

“No optics is the best optics”!?

Y b t Yes, but …In principle possible - all in vacuum, working

with non-modified “white” or “pink” beam.

However, not very useful. We may need e.g.

monochromatisation, focussing, ... .

Page 7: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

A whole zoo of optical elements

• slits, pinholes• filters, windows• mirrors (reflectivity based)• beam splitter monochromators (crystals)

h / ll / l ( l• monochromators/collimators/analysers (crystals,multi-layers – often also called “mirrors”)

h l ( h d l i ) ( l )• phase plates (phase retarder, polarizer) (crystals)• lenses, zone plates

bi d l t (ML ti B F l l )• combined elements (ML gratings, Bragg-Fresnel-lenses)• etc.

Mirrors and monochromators, collimators, analysers flat, but also bent for collimation, focussing, image f at, ut a so nt for co mat on, focuss ng, mag

magnification, ...

Page 8: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Main physical effects used in X-ray optics were discovered inthe first years starting from the discovery of X rays bythe first years starting from the discovery of X-rays byC. W. Röntgen:

absorption (Röntgen 1895/96 filters)absorption (Röntgen 1895/96 filters)Bragg-diffraction (Laue 1912 monochromators, etc.)specular reflection (Compton 1922 mirrors)refraction (Larsson, Siegbahn, Waller 1924 later lenses)

P ti f d bl d t l tProperties of double and many-crystal set-ups:Jesse W. M. DuMond, Physical Review, 52, 872-885 (1937)DuMond graphs dispersive and non dispersive set ups DuMond graphs, dispersive and non-dispersive set-ups, channel cut crystals (later invented as “Bonse-Hart-camera”), four crystal spectrometer (later invented as “Barthels four crystal spectrometer (later invented as Barthels monochromator”), etc.

B d lBut - many newer developments

Page 9: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Quite a lot of literatureQ

Overviews:

Tadashi Matsushita, X-ray Monochromators, in Handbook on Synchrotron Radiation, Vol. 1, ed. E. E. Koch, North-Holland P bli hi C 1983Publishing Company, 1983

Dennis M. Mills, X-Ray Optics for Third-Generation Synchrotron Radiation Sources, in Third-Generation Hard X-ray Sources, ed. Dennis M. Mills, John Wiley & Sons Inc., New York, 2002,

Page 10: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Short remark concerning beam dimensionsShort remark concerning beam dimensionsShort remark concerning beam dimensionsShort remark concerning beam dimensions

Few years ago – micro-beams were modern,

now – nano-beams are in voguenow nano beams are in vogue.

But - we need all kind of beams:

large beams (decimetre sized) g ( )and small ones (nanometre sized),

“parallel” divergent and focussed beamsparallel , divergent and focussed beams.

Page 11: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Beam dimensions – example: paleontologyp p gy

Examples from Paul Tafforeau

Page 12: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption
Page 13: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption
Page 14: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Nearly 4 orders of magnitude in dimension

Without scanning

Without magnificationWithout magnification

Multi scale experiments!

Page 15: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Further large scale objects: the monochromator crystals

For their tests we like to use:wide beams if possible at least 10 x 45 mm2 (V x H)wide beams, if possible at least 10 x 45 mm2 (V x H),with a “good” spatial resolution ~ 1 μm

The above field of view and resolution needs sensors with:10,000 x 45,000 pixels, this is 450 Mega pixels

Not yet on the market (?)Not yet on the market (?)

Page 16: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

but also by: filters + 2. Monochromators2. Monochromators100

E = 8 keV

100

E = 8 keV

source spectrum + scintillator screen

response spectrum (P l T ff /ID19)

10-2

10-1

forbidden area 10-2

10-1

forbidden area

(Paul Tafforeau/ID19)

10-3

10-2

d re

flect

ivity

R = 1

ors)

10-3

10-2

d re

flect

ivity

R = 1

ors)

10-4

10

Inte

grat

ed

High-ZLow-Zn

ML

's

d M

L's

Ge111

(Mir

ro

10-4

10

Inte

grat

ed

High-ZLow-Zn

ML

's

d M

L's

Ge111

(Mir

ro

10-5 Crystals

ML's

h-re

solu

tion

epth

-gra

dedSi

111

10-5 Crystals

ML's

h-re

solu

tion

epth

-gra

dedSi

111C*

111

10-6

10-6 10-5 10-4 10-3 10-2 10-1 100hi

gh de

Be110

10-6

10-6 10-5 10-4 10-3 10-2 10-1 100hi

gh de

Be110

Ch. Morawe

E/EHigh resolution 10-8 and below

Page 17: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Bragg diffracting X-ray optical elements like

M f t d f di l ti f t l

gg g y pmonochromators, analysers, etc.

Manufactured from dislocation free crystals.Mostly used: Si, Ge, C* (locally dislocation free diamond).

We mainly use silicon.

They must be tailored into monochromators etc.

Orientation cutting lapping polishing and etchingOrientation, cutting, lapping, polishing and etching.

Strain free crystal preparation.

Accurate and stable mounting.

Adequate cooling schemeAdequate cooling scheme.

Page 18: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Crystal laboratory:Crystal laboratory:

Manufacturing of nearly all perfect Si (and few Ge) crystal Si (and few Ge) crystal monochromators & analysers, etcfor all ESRF beam lines, CRG b li d t l beamlines and external laboratories.Silicon pieces are made from float Silicon pieces are made from float zone silicon ingots with 100 mm diameter (Wacker).More than 1.5 tons of silicon single crystal material has been processed in more than twenty yearsin more than twenty years.

Example manufacturing crystal monochromators and analysersmonochromators and analysers

Page 19: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Which types of monochromators are used?yp

Page 20: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Single crystal monochromators -beam splitter monochromators

white beam white beam white beam

monochr. beam 2monochr. beam 1

Double crystal monochromators

white beammonochr. beam

Reflection (Bragg) and t nsmissi n (L ) transmission (Laue) geometry used

Page 21: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Single crystal monochromators -beam splitter monochromators

white beam white beam white beam

monochr. beam 2monochr. beam 1

Double crystal monochromators

Reflection (Bragg) and t nsmissi n (L )

white beam monochr. beam

transmission (Laue) geometry used

Page 22: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Few theory and definitionsFew theory and definitions

Reflectivity (and transmissivity) curve of a crystalplane RTheory

Plane & monochromaticincoming wave,

plane monochromatic

waveDarwin width

R

R+T+A=1

incoming wave,varying the angle of incidence

counting the diffracted photons

width

Rocking curveReal situation - experimentConvolution (autocorrelation) of

R T A 1

any wavereflectivity (or transmissivity) curve

with other reflectivity curves,or/and wavelength (energy) g ( gy)

distribution,or/and divergence distribution

(instruments/apparatus function)( pp f )

Page 23: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Numerical example (using XOP):d bl h di i ( )

Numerical example (using XOP):d bl h di i ( )double monochromator non-dispersive (+,-)double crystal set-up in Bragg casedouble monochromator non-dispersive (+,-)double crystal set-up in Bragg case

two 111-Si reflections

wh 0 8

1,0

two Si 111 crystals

0 8

1.0

Darwin curveSi 111, 60keV, 10mm thick plateSi 111, 60keV, 5cm thick plate

gg

wh

wh

0,4

0,6

0,8

refle

ctiv

ity

0.4

0.6

0.8

refle

ctiv

ity

emat

ical

Bra

gpo

siti

on

0

-1,0 -0,5 0,0 0,5 1,0 1,5 2,0 2,5 3,0 3,5 4,0 4,50,0

0,2

-1.0 -0.5 0.0 0.5 1.0 1.5 2.0 2.50.0

0.2 kine

angle - B (arc seconds)angle - B (arc seconds)

However, in operation known since: C. G. Darwin, However, in operation – mostly fixed angleThe theory of X-ray reflection,

Phil. Mag. 27, 315, 675 (1914)

Page 24: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Reflectivity curves, with stronger absorptionReflectivity curves, with stronger absorptiony g py g p

Prins-Darwin or reflectivity curveSi 111, 8keV, 5cm thick plate

0 8

1,0 Si 111, 8keV, 5cm thick plate

w

0,6

0,8tiv

itywh

0,4refle

ct

0,0

0,2

-5 0 5 10 15 20,

angle - B (arc seconds)

How to measure it? Not so easy! See later.

Page 25: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Double crystal monochromatorsDouble crystal monochromators

Incident and exit beams have the same directionhave the same direction

In working position: RR()

fixed angle (mostly);

multiplication of two R

2

multiplication of two reflectivity curves

Page 26: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Two variantswo var ants

Fixed exit monochromator- more than one movement

necessary

Page 27: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Two variantswo var ants

Fixed exit monochromator- more than one movement

necessary

Page 28: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Two variantswo var ants

Fixed exit monochromator- more than one movement

necessary

Channel-cut monochromator- NOT fixed exitNOT fixed exit- naturally aligned- weak link plus piezo

movement for detuning etc.

Page 29: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Two variantswo var ants

Fixed exit monochromator- more than one movement

necessary

Channel-cut monochromator- NOT fixed exitNOT fixed exit- naturally aligned- weak link plus piezo

movement for detuning etc.

Page 30: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Two variantswo var ants

Fixed exit monochromator- more than one movement

necessary

Channel-cut monochromator- NOT fixed exitNOT fixed exit- naturally aligned- weak link plus piezo

movement for detuning etc.

Page 31: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

“Generic” cryo enically Generic” cryogenically cooled channel-cut double

crystal monochromator

Pusher

y

no fixed exit

high heat load applications Pusher mechanism

Steel flexure

high heat-load applications

Channel-cut crystal

Crystal assembly (simplified for visibility)

Page 32: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Possible problem – “higher harmonics”p g2dnh’,nk’,nl’ sinB = nif (h,k,l)=(nh’,nk’,nl’)

Si (2n,2n,0), = 1.6Å, = 0.8Å, etc.

Refraction correction (middle of the reflection domain):

BhB0 sin,sin

h0

20

0 12sinV2

Fr

Refraction correction (middle of the reflection domain):

0Buc 2sinV2

Page 33: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

R d ti f hi h h m i s (if mi s m b s d)Reduction of higher harmonics (if no mirrors may be used)monochromator detuning

d d At detuned position(slightly misaligned)

S ll b d i Smaller band in angle and energy

Page 34: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Synchrotron optics: Multilayer high flux monochromators• Two bounce optics• 100x larger bandwidth compared with Si(111)• Harmonics suppression due to refraction and filling factor

Ch. Morawe – SPring-8 11.09.07

Page 35: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

How may I change the beam dimension,y gthe beam divergence, th l ti ?the energy resolution?

Page 36: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

3. Some properties of asymmetrical 3. Some properties of asymmetrical flfl

3. Some properties of asymmetrical 3. Some properties of asymmetrical flfl

p p yp p yreflectionsreflections

p p yp p yreflectionsreflections

Up to now we looked at symmetrical cases of Up to now we looked at symmetrical cases of Bragg diffraction

symmetrical Bragg case

(reflection case)

symmetrical Laue case

(transmission case)

– angle between lattice planes and surface

(reflection case) (transmission case)

Page 37: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

With asymmetric reflections - possibilities to change y p gthe beam width and the divergence

for a single crystal reflection

Lin0K

whin

in

hK

Lout

whout

Page 38: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Of course, the same works also other way around.

So we have possibilities to act on the beam dimension (expansion, compression), as well as on

h b d ( ll l )the beam divergence (smaller, larger)

LouthK

whout

out

0K

Lin

whin

Page 39: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

But all is related and things have their price

L 0Kwh

in

Lin 0K

hK

Loutwh

out

0B)i ()sin(b

Asymmetry factor:

hB )sin(

w out = |b| w inThis example: >0, |b|<1: whout = |b| wh

in

Relation to symmetrical reflections

pLin > Lout and wh

in < whout

w in L = w out L = constant reflectionswh

in = |b|-1/2 whsym

whout = |b|1/2 wh

sym

wh Lin = wh Lout = constant

right asymmetry (<0) – less divergence possible to obtain h | | hg p

Page 40: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Some “philosophy”p p yWith flat crystals we may change the divergence.We may decrease (or increase) it. Not “more parallel”, y ( ) p ,but less divergent! This is collimation*). Focussing needs convergent beams. We can not focus

i h fl l i l i l I k i h b with flat crystals in a classical way. It works with bent crystals. Often other X-ray optical elements are more efficient for this (future lectures?!)

*) The word "collimate" comes from the Latin verb collimare,

efficient for this (future lectures?!).

The word collimate comes from the Latin verb collimare, which originated in a misreading of collineare, "to direct in a straight line". (Wikipedia)

Page 41: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

BUT BUT …wh

in Lin = whout Lout = constant

This is too simple, hand-waving “derivation”. We need an additional dimension for the h phase space.

Besides size and anglel l h ( ) i d dalso wavelength (or energy) is needed

L t t t f th b iLet us start from the basics

Page 42: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

0 = B + - in K

0 B in

h = B - + out

0Kh

t

From electrodynamics (and dynamical diffraction theory)

n

BB

dynamical diffraction theory) we know that: 0K

hK

0h

hKK 0h

For the wave vectors outside the crystal:0h

But for the tangential components - continuity:

tt0ht hKK

And remember, wave vectors depend on wavelength: )(fK , p g )(

Page 43: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

For small in, out and K we obtain (for Bragg and Laue case!):

K

Ksin

)cos()cos(sinsin||

B

BBin

B

Bout

The divergence in and polychromaticity K/K of the incomingbeam contribute to the divergence out of the outgoing beam

BB

beam contribute to the divergence out of the outgoing beam

An increased divergence out of the outgoing beam (with respect t th t if th i i b ) s: to that if the incoming beam) means: the source is virtually closer, or the source size is virtually larger, or the angular source size is virtually larger.

Special case 1

Monochromatic divergent incoming radiation

arg r, or th angu ar sourc s z s rtua y arg r.

Monochromatic, divergent incoming radiation

K = 0, in 0 out = |b| in

t ior whout = |b| wh

in

Page 44: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Special case 2

P l h ti ll l i i di tiPolychromatic, parallel incoming radiation

K 0, in = 0 K)cos()cos( BB

K)sin( Bout

Remember, “our” beams often are rather close

2.1. out = 0 if cos(B - ) = cos(B + ) if (sym. Bragg case!)

to plane waves, but rather polychromatic

Only in the symmetric Bragg case the beam divergenceis conserved for a polychromatic beam!!!Only in that case coherence is conserved!!!Only in that case coherence is conserved!!!Only in that case focussing is not perturbed!Only in that case highest geometrical resolution possible!

2.2 out 0 for all other cases

A divergent, polychromatic beam is transformed in a d l h b !even more divergent, polychromatic beam!

Page 45: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Source size and angular source size are crucial Source size and angular source size are crucial parameters with respect to the character of the wave “seen” by the sample.

angular source size ( = s/p)p

not source divergence!!ps δ

The angular source size is important for further physical properties:physical properties:

the geometrical resolution for imaging,the transversal coherence lengththe transversal coherence length,the demagnification limit of a “lens”.

Page 46: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Image blurring due to non-zero source size

angular source size: δ = s/p

qps δ

geometrical resolution: ρ = q s/p = q δ

s δqp

s δ

Spatial coherenceSpatial coherenceTransversal coherence length: lT = ½ λ p/s = ½ λ/δ

Page 47: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Magnification, demagnification, focussing properties/quality

G t i l d ifi ti Diff ti li it d f iGeometrical demagnification,source size limit:

/ δ

Diffraction limited focusing:ρDL = 1.22 λ / sinα

s ρ

ρG = q s/p = q δ

s ρ

p q(graph: J Susini)(graph: J. Susini)

Page 48: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

4 Shortly about high energy resolution4 Shortly about high energy resolution4 Shortly about high energy resolution4 Shortly about high energy resolution4. Shortly about high energy resolution4. Shortly about high energy resolution4. Shortly about high energy resolution4. Shortly about high energy resolution

One way: One way: Sophisticated many crystal set-ups.

Example ID18:A two-step collimation with low-index

l ll asymmetric reflections followed by a two-step angular analysis with high-index asymmetric reflections reflections.

Idea: M.Yabashi, K.Tamasaku, S.Kikuta, and T.Ishikawa, Review of Scientific Instruments, 72, 4080 (2001).

Page 49: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

ID18 ESRFID18 ESRF Alexander Chumakov ID18/ESRF

High resolution optics for Nuclear Resonance Scattering“0.5 meV” monochromator (∆E/E ≈ 3.5·10-8)

(theoretically expected performance)

High-resolution optics for Nuclear Resonance Scattering

(theoretically expected performance)

31

divergence: 65 nano-radacceptance: 130 nano-rad

vertical size: 0.6 mmdivergence: 2 radvertical size: 0.6 mm

31 mm

23

divergence: 2 rad divergence: 2 rad

14

1st crystal: Si(400)B = 18.469º

t |b| 0 18

2nd crystal: Si(400)B = 18.469º

t |b| 0 18

3rd crystal: Si(12 2 2)B = 77.533º

t |b| 9 8

4th crystal: Si(12 2 2)B = 77.533º

t |b| 3 2asymmetry: |b| = 0.18in = 5.4ºout = 31.6ºangular acceptances:in = 20 rad

asymmetry: |b| = 0.18in = 5.4ºout = 31.6ºangular acceptances:in = 20 rad

asymmetry: |b| = 9.8in = 27.6ºout = 2.7ºangular acceptances:in = 0.72 rad

asymmetry: |b| = 3.2in = 35.4ºout = 10.4ºangular acceptances:in = 1.3 radin

out = 3.6 radfootprint: 6.4 mm

in out = 3.6 radfootprint: 33 mm

in out =7 radfootprint: 41 mm

in out = 4 radfootprint: 3.3 mm

Page 50: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Other possibility – back scattering geometry(Bragg angle close to 90 deg)

with high order reflections (large h k l)

= 2dhkl sinB ∆ = ∆ · 2dhkl cosB

∆ ∆E/E ∆ /∆= ∆E/E = ∆/tanB

) f 10 8 d b) d [ t () 0]

Silicon @ 20KeV, h=k=l=13, (E/E) ~10-8E ≈ 0.5 meV,

a) → a few 10-8 rad b) → deg [cotg() → 0]

@ , , ( ) ,

ID16, ID28 Sample

analyserp

Detectormonochromatorsource

Page 51: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

5. How high crystal quality and how to 5. How high crystal quality and how to

5. How high crystal quality and how to 5. How high crystal quality and how to

g y q yg y q ymeasure it?measure it?

g y q yg y q ymeasure it?measure it?

Crystal quality - limit in high energy resolution, …(?)

I fl h ti i lit Influence on coherence preservation, image quality, focussing efficiency, ...

Page 52: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption
Page 53: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

∆d/d= 5x10-9

Page 54: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Crystal interferometers

Page 55: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Diamonds at the ESRFDiamonds at the ESRFFrom the very beginning of the ESRF used as h l t d h tphase plates and monochromators.

Now locally dislocation- and stacking fault free Now locally dislocation and stacking fault free material available.

Which is the level of local residual strains?

Page 56: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Future MX BL ID30A (MASSIVE)

~100 μm215 2 100 μm~15 μm2

56

Page 57: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

X-ray diffraction topographyWhite beam topograph

in transmission

(work with Fabio Masiello)

110-oriented plate

supplier: Paul ppBalog/Element Six

Dislocation free areas of 11 3 mmDislocation free areas of 6x4mm2 and more!!!

Locally crystal quality close to that of silicon

11.3 mm

Locally crystal quality close to that of silicon, quantitatively confirmed by double crystal topography

But are we able to measure weak strains quantitatively?

Page 58: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Quantitative analysis strain analysis110-oriented crystal plate

effective misorientation map

Q y y

effective misorientation map basing on one topograph

20keV Si [880] C* [660] 20keV, Si [880] C [660], detection limit: δθ > 8·10-9

The effective misorientation is The effective misorientation is of the order of 4 × 10−8 for a

region of interest of0 5 × 0 5 mm2 and × 10-80.5 × 0.5 mm2 and

1 × 10−7 in a region of1 × 1 mm2

Sample is slightly bent due to the non-homogeneous

dislocation distribution!dislocation distribution!work with Fabio Masiello

Page 59: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

6. Plane or divergent, monochromatic or l h ti

6. Plane or divergent, monochromatic or l h ti polychromatic wavespolychromatic waves

Two basic questions:What are “plane” or “divergent” waves?

Wh “ h i ” “ l h i ” “ hi ”

w qu

What are “monochromatic”, “polychromatic”, “white”beams/waves?

For our monochromator and/or single crystalline sample!

Reminder of basic physics:Reminder of basic physics:Plane wave – infinite extend, wave front is plane, one wave vector perpendicular to it, delta-function in k-space.Monochromatic wave – wave train of infinite length, infinitely sharp spectral line, delta-function in ω-space.They do not exist in nature!!!They do not exist in nature!!!

Page 60: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

The full width at half maximum of the reflectivity curve,y ,

good reference for our sample, monochromator, ... , to define the character of a wavedefine the character of a wave

R()FWHM in the angular space:

P h h h 2

R()

wh

g p

whh h

B

h

2 0

sin

FWHM in the wavelength space: R()

wh

w wh h B cot

Page 61: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Example of a typical crystal/monochromator reflection:

silicon, 111 reflection, Bragg case, thick crystal

energy wh wh

/energy wh wh /

8 keV 7.6 arcsec 1.5·10-4

20 keV 2 9 arcsec 1 5 10-420 keV 2.9 arcsec 1.5·10-4

Those are to be compared with source properties:

wave length spread of the source ()wave length spread of the source ()

angular source size ( = s/p)ps

not source divergence!!ps δ

Page 62: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

relative wave length spread of the source (E/E)

FWHM in the wavelength space hw<<

“ h ” “monochromatic” wave

angular source size = s/p

<< FWHM in the angular space hw

“plane” wave

Page 63: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Practical examples:

relative wave length or energy spread of the source

source

source

Si 111 double mono 2·10-4

energy

8 keV

wh/

1.5·10-4

laboratory (e.g. CuK1) 3·10-4

white beam 1···10

20 keV 1.5·10-4

SR–white beams: >>> wh

really polychromatic

”monochromatic” beam (SR or laboratory): <?> wh

often not monochromatic(for all reflections narrower than the 1.5·10-4 for silicon 111)

special effort is necessary to approximate “monochromaticity”p y pp y

Page 64: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Practical examples:

angular source size ( = s/p)

source source size s source dist D δsource source size s source dist. D δ

class. lab tube 400 µm 0.4 m 1·10-3 3.5 arcmin

f t b 5 1 1 10 5 1

energy

8 keV

wh

7 6 arcsecµ-focus tube 5 µm 1 m 1·10-5 1 arcsec

SR 100 µm 150 m 6.7·10-7 0.14 arcsec

7

8 keV

20 keV

7.6 arcsec

2.9 arcsec

SR 50 µm 75 m 6.7·10-7 0.14 arcsec

laboratory: >< wh divergent & quasi plane waves possible

SR - ESRF: < wh quasi plane wave (mostly)

Source divergences > angular source sices

E F h q p (m y)

g g

Page 65: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

For your curiosity:y yFirst published (direct) measurements of

fl i i fl i i reflectivity curvesreflectivity curves,(Not rocking curves! Those were measured earlier),g

the ones that we are able to calculate since Darwin’s first dynamical theory published in 1914, was in???

1962

first dynamical theory published in 1914, was in???

nearly 50 years after Darwin’s results!!!nearly 50 years after Darwin s results!!!

C. G. Darwin, The theory of X-ray reflection, Phil. Mag. 27, 315, 675 (1914)Charles Galton Darwin (1887-1962) grandson of Charles Darwin

Page 66: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

How can we measure a reflectivity How can we measure a reflectivity curve???

Not trivial. One needs two ingredients.

1. Narrow instruments function

in angular space – asymmetrical reflectionsg p ymm f

in wavelength space – high-resolution mono.

2. Crystals of good quality. They became available with development

of electronics, later micro-electronics and opto-electronics

Page 67: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Double (or triple) crystal monochromator collimator Double (or triple) crystal monochromator-collimator with one asymmetrical Bragg reflection

Page 68: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

1st experimental reflection curves

=-4.48

=0

=4.48

111-reflections of Ge, different asymmetriesy

CuK1-radiation, triple crystal set-up, silicon double monochromator

R. Bubáková, Czech. J. Phys. B12, 776 (1962), J y , ( )

Page 69: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

B th th p b bl fi st p blish d By the way – the probably first published measurements in a double crystal set-up with an asymmetric monochromator/collimator crystal asymmetric monochromator/collimator crystal were about X-ray diffraction topography in 1952.

W. L. Bond J. Andrews, Structural Imperfections in Quartz Crystals, p yAm. Mineral. 37, 622-632 (1952)

This technique was later developed further to the “Plane” Wave Topography,

t d t t t l ll t i fi ldto detect extremely small strain fieldsin nearly perfect crystals.

Page 70: XX-X-ray opticsray opticsMain physical effects used in X-ray optics were discovered in the first years starting from the discovery of X-rays by C. W. Röntgen: absorptionabsorption

Thank you for your Thank you for your tt ti !attention!