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Which are their properties? How is it produced? What is it? Where is it produced? How and why it is used? What is foreseen for the future? Settimio Mobilio Dipartimento di Fisica Universita’ Roma TRE

What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

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Page 1: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Which are their properties? How is it produced? What is it?

Where is it produced?How and why it is used?

What is foreseen for the future?

Settimio MobilioDipartimento di FisicaUniversita’ Roma TRE

Page 2: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Synchrotron Radiation

Electromagnetic Radiation Emitted by an acceleratedcharge moving with relativistic a speed v ~ c

Today: radiation emitted by relativistic electrons (positrons) in a storage ring

Future: also radiation emitted by relativistic electrons (positrons) in a linear accelerator (LINAC)

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References

Handbook of Synchrotron RadiationElsevier (North Holland) editor

“Synchrotron light”Springer-Verlag Compact Disk 2000

http://xdb.lbl.gov/

1. G. K. Green, “Spectra and Optics of Synchrotron Radiation,” in Proposal for National Synchrotron Light Source, Brookhaven National Laboratory, Upton, New York, BNL-50595 (1977).

2. H. Winick, “Properties of Synchrotron Radiation,” in H. Winick and S. Doniach, Eds., Synchrotron Radiation Research (Plenum, New York, 1979), p. 11.

3. S. Krinsky, “Undulators as Sources of Synchrotron Radiation,” IEEE Trans. Nucl. Sci. NS-30, 3078 (1983).

4. D. Attwood, Soft X-Rays and Extreme Ultraviolet Radiation: Principles and Applications (Cambridge Univ. Press, Cambridge, 1999); see especially Chaps. 5 and 8.

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S.R. Energy Range

Synchrotron ligh sources

Page 5: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Synchrotron Radiation Properties

1. Continuous spectrum from infrared to hard X-ray2. High intensity 3. Narrow angular collimation4. High degree of polarization5. Pulsed time structure6. Partially coherent (for the moment)7. Quantitatively evaluable.

High Brilliance

Storage RingUltra-high vacuum environment

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Brilliance

Ω

SourceA (mm2)

e-

Focusing device

Mirror

ImageN (Photons/sec)

( ) ( )⎟⎟⎠

⎞⎜⎜⎝

⎛Ω⋅

=ban%.radm.mm

sec/PhotonsA

NBrilliance1022

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Brilliance of the synchrotron radiation

Comparison between the average brilliance of storage ringsof different generations.

XFEL

III Generation

I and II Generation

X-ray tubes

Page 8: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Schematic view of a Storage Ring

• Bending magnets (main dipoles) • The Radio Frequency cavity • Straight sections Insertion devices (undulator)• Focussing and de-focussing magnets (quadrupoles)

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Synchrotron light from a storage ring

Undulator

injector

R.F. cavity

1 m

Wiggler

Bending magnet, BM

BM

BM BM

BM

BM

BM

BM

Synchrotron light

Synchrotron light

Beamline

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Origin of Synchrotron RadiationA classical accelerated

charge emits e.m. radiation symmetrically with respect to

the acceleration

θp0sinωt

v << cThe radiation angular distribution of non-relativistic electrons hasthe shape of a tire orbiting at the same velocity of the electron bunch

v << cThe radiation angular distribution of non-relativistic electrons hasthe shape of a tire orbiting at the same velocity of the electron bunch

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Origin of Synchrotron Radiation

θ

v ~ 0

v ~ c

Lorentz tra

nsform

e

eL αβγ

ααcos11sinsin

+=

E

E

αL

αe

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Angular distributionA relavitistic accelerated chargeemits e.m. radiation mainly into

the direction of the speed

Cone aperture

mradEcm1 2

0 ≅=γ

Electron orbit

Acceleration

v << c

v ≅ c

Electron orbit

Acceleratione-

e-

Θ ≅ m0c2/E= 1/γ radm0 = electron mass

v = electron velocityE = electron energyc = velocity of light

v

v

Page 13: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Synchrotron Radiation Sources

Bunch of relativisticelectrons

Light

N

S

Bending magnet

e-Insertion device

Page 14: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Spectral distribution of synchrotron radiation

10-1 100 101 102 103 104 105E (eV)

Infrared Visible Ultraviolet Soft X-ray Hard X-rays

1012

1013

1014

1015

λc

105 104

Phot

on fl

ux(P

hoto

ns /

s ·m

rad

(0.1

% b

and

pass

))

λ (Å) 102 101 100 10-1103

EC

Continuousfrom I.R. to X-ray

Specific shape

Ec critical energy= 3hγ3c/4πR

Page 15: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Spectral distribution of synchrotron radiation as a function of the of critical energy of the storage ring.

εc=0.58keV

εc=1.4keVεc = 3hγ3c/4πR

λc = 4πR/3γ3

The power emitted at wavelengths lower than λc is equal to the power emitter at wavelengths higher than λc

Page 16: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Origin of the broad spectral distribution

The detector receives the radiation for a short time

The detector records the radiation emitted along the arc 2/γ

the duration of the pulses is non zero (τ)

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Polarization

Mainly linear In the plane of

the orbit

Two polarization component±π/2 out of phase

E

There is a second componentperpendicular to

the orbit

Left and right circular polarization

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Time Structure

bunches

Bunch time length 10 – 100 ps

t

I

e- e-e- e-

Repetition rate: Maximum time distance = period of the orbitMinimum time distance = period of the RF

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Angular emission from a Bending magnet

• The orbit is circular• The radiation is emitted tangentially• It is collected in a horizontal slit (S) of width, w, at a distance, D.

∆θ = S/D

In the vertical direction the natural collimation preserved

In the horizontal direction the natural collimation is lost

Insertion Devices

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Emission view

Top view

Electron orbital plane

Side viewΨ ≅ 1/γ (≈10−4 mrad)

Page 21: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Angular and wavelength distribution of synchrotron radiation

The power radiated by an electron in a unit wavelength intervalcentred at λ in a unit vertical angular cone centred at ψ is given by:

1. R is the bending radius of the electron orbit 2. K1/3 and K2/3 are modified Bessel functions of the second kind3. λc is the so called critical wavelength

In pratical units:λc (Å)= 4/3 π R γ-3

ξ= (λc/2λ) [1+ (γψ)2]3/2 λc = 5.59 R(m) Ε-3 (GeV)

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Angular and wavelength distribution of S.R.

λc = 4/3 π R γ-3

ξ= (λc/2λ) [1+ (γψ)2]3/2

λc(Å)= 5.59 R(m) Ε-3 (GeV)

Note that:• the wavelength dependence is only on the ratio λc/λ• the angular dependence is only on the product γψ

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Two polarization component±π/2 out of phase

In the plane of the orbit

Perpendicular tothe orbit

Left and right circular polarization

above and below the orbit

Polarization

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Behavior of the parallel and perpendicular componentfor different λ/λc

The integration over all wavelengths gives:I// = 7/8 Itotal

I⊥ = 1/8 Itotal

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Insertion devicesMagnetic field structures

Force the electrons to move along particular orbits

N S N S N S

N S N S NSe-

∆t

WigglersUndulators

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Insertion devices

Magnetic field structures Force the electrons to move

along particular orbits

∆Ψ = 1/γ

Ψ

Ψ2αR

t+∆t

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Wiggler Condition

BBmceK uu λλ

π934.0

2==Dimensionless parameter K

[cm][T]In a wiggler K>>1∆Ψ = 1/γ

In a wiggler the angularoscillations of the electrons α=K/γ are much wider than the natural opening angle

∆ψ=1/γ

Ψ

Ψ2αR

t+∆t

•No interference between the emission from different poles•Total emission is the sum of the emission from each pole

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Wigglers Emission

E = 1.5 GeV I = 100 mA1013

1012

1011

10 102 103 104 105

Wiggler 1.85 T

Bending magnet

Wiggler 6 T

Photon energy (eV)

Phot

on F

lux

Higher magnetic field higher critical energy

Radiation from the poles increases

the total emission

Multipole magnet made up of a periodic arrangement of N

magnetswhose magnetic field forces

electrons to wiggle around the orbit

Wigglers have higher critical energy enhance the X-ray emission

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Undulator

Page 30: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Undulators conditionAn undulator is similar to a

wiggler with a K < 1

The wiggling angle is smaller than the photon natural

emission angle 1/γ

Interference effects are important

⎟⎟⎠

⎞⎜⎜⎝

⎛++= 22

2

2 21

2θγ

γλλ Ku

Observing the radiation at an angle θ from the axis

constructive interference occur at the wavelengths

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Undulator fundamental frequency

An undulator as seen in the laboratory reference system

λ0 = L/nMagnetic pole periodicity

L

n = number of periods

λ’0 = L/nγ = λ0 /γ

The undulator as seen from the electron

Relativistic contraction

Further reduction of the light periodicity due to the Doppler effect

Doppler shift2

00

221

γλ

=γγ

λ=λ

Spectrum

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Undulator harmonics

⎟⎟⎠

⎞⎜⎜⎝

⎛++= 22

2

2 21

2θγ

γλλ Ku

Also harmonics λ/n are emitted

On the axis (θ=0) only odd harmonics are emitted

nN1

=∆λλ

Harmonics bandwidth

Values of 10-2 are easily obtained for the fundamental

The radiated field adds coherentlyThe intensity increases as N2

while in a wiggler it increase as 2N

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The angular distribution is concentrated in a narrow

cone both in horizontal and vertical directions

N S N S N S

S N S N S N

N S N S N S

Top view

Side view

γn1

γn1

Undulator angular emission

nNnNK 112/1

43

2

2

r γγπσ ≈

+=

Radiation from an undulator: typically N = 50

The natural emission cone is always smaller than 1/γ

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Spectral brilliance

For experiments that require a small angular divergence and a small

irradiated area, the figure of merit is the beam brillianceB which is the photon flux

per unit phase space volume, often given in units of photons·s–1·mr–2·mm–2·

(0.1% bandwidth)–1

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Beamlines

Page 36: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Synchrotron Radiation Facilities around the world

About 50 facilities in the worldhttp://www-als.lbl.gov/als/synchrotron_sources.html

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Synchrotron Radiation Facilities in Europe

About 20 Facilities, most dedicated, few parasitic

III Generation FacilitiesPolicy in Europe

ELETTRA in ItalyBESSYII in Germany

SLS in SwitzerlandDIAMOND in UKSOLEIL in France

ALBA in Spain

At home: Medium energy (~ 2GeV) S.R. For high brilliance in soft X-ray

And brilliance in hard X-ray

GermanyDORIS III in Hamburg

European Synchrotron Radiation Facility ESRF in GrenobleFor High Brilliance in the hard X-ray region

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European Synchrotron Radiation Facility -ESRF

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European Synchrotron Radiation Facility -ESRF

Members' Contribution to the budget: 27.5% France25.5% Germany 15% Italy14% United Kingdom4% Spain4% Switzerland6% Benesync

(Belgium,Netherlands)4% Nordsync

(Denmark, Finland,Norway, Sweden)

Additional contributions1% Portugal1% Israel1% Austria0.6% Poland (from July 2004)0.44% Czech Republic0.2% Hungary

Page 40: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Parameters of the ESRF

Energy 6GeV

Circumference 844m

Current 200 mA

Bending Magnet Radius

24.95m

RF frequency 352.2MHz

Harmonic number 992

Critical Energy 19.6 KeV

Undulator 1st

Harmonic14 KeV

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ESRF Achieved Brilliance

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ESRF Brilliance

Page 43: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

ESRF Experimental Hall

Undulator BL 34

Bending Magnet BL 3

CollaboratingResearch groupBeamlines 13

Page 44: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Science at ESRFMagnetism:

Separation of S and L contributionContribution of different electronic shells

Surfaces:Structure of surfaces and overlayersSurface magnetism

X-ray InelasticScattering:

Lattice dynamics &Electronic States

Life Science:Protein CrystallographyTime resolved crystallography

Chemistry:High resolution crystallographyMicrocrystalsCatalysis

High Pressure:Phase diagram up to 150 Gpa

Medicine:Microbeam therapyTomographyAngiography

Industrial:High resolution strain ( 10µ 10-5 strain)Trace element analysis (LLD 106 at/cm2)

Imaging: Phase Contrast ImagingSpeckel

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Energy: 2 – 2.4 GeVCurrent: 300 mACritical Energy: 3.2 KeV

Spectral Range: 10 eV – 10 KeV

ELETTRA

Undulator first Harmonic: 200 – 800 eV

Brilliance: 1019 photons/s/mm2/mrad2/0.1%bw

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Beamlines at ELETTRA

13 Operating Beamlines19 Experimental Stations

2 are under commissioning

4 More in the future

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Science at ELETTRA

Surfaces/MoleculesChemical Reactions

Microscopy

Photoemission

Magnetism

Dichroism

Diffraction

CrystallographyProtein Crystallography

MammographyPhase Contrast Imaging

Medical Physics

Microstructure Fabrication for:OpticsMagnetic nano-patteringMicro machine devices

Lithography

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Beamlines versus science at ELETTRA

ESCAMicroscopyNanoSpectroscopySuperESCASpectro Microscopy

Surface Diffraction ALOISAGas PhaseVUV PhotoemissionBEAR

SYRMEP (Medical beamline)

PolarBach ( Beamline for Advanced Dichroism )APE

X-Ray DiffractionSmall Angle X-Ray Scattering

XAS

LILIT ( Lithography)Deep-etch Lithography

Chemistry Surfaces

BiologyMaterial Science

Magnetism

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DAFNE

Page 50: What is it? How is it produced? Which are their properties? Where … · 2020-01-16 · Which are their properties? How is it produced? What is it? Where is it produced? How and why

Free Electron Laser

FEL are tunable, coherent, high powerradiation, currently spanning wavelengthsfrom millimeter to visible and potentially

ultraviolet to x-ray.

It has the optical properties characteristic of conventional lasers such as high spatial coherence and a near diffraction limited radiation beam. It differs from conventional lasers in using a relativistic electron beam as itslasing medium, as opposed to bound atomic or molecular states, hence the term free-electron

First laser: Madey 1977-78 at Stanford(10µm)

Existing Facilities/Experiments: mainly in IR 1- 100 µm(about 30) few in visible - UV

Standard Linac

S.R.

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SASE Free Electron Laser Scheme

In a long undulator the SR emission is self amplifiedIn a very long undulator saturation may be reached At a level 7 order of magnitude above the S.R. level

Key points: electron beam emittanceundulator characteristics

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More on SASE Free Electron Laser Scheme

The electron beam and thissynchrotron radiation travellingwith it are so intense that the electron motion is modified by the electromagnetic fields of its ownemitted synchrotron light. Under the influence of both the undulator and its own synchrotronradiation, the electron beam beginsto form micro-bunches, separatedby a distance equal to the wavelength of the emitted radiation.

These micro-bunches begin toradiate as if they were single particles with immense charge. The process reaches saturationwhen the micro-bunching hasgone as far as it can go.

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FEL Radiation Properties

FEL SpontaneousEmission

ExistingUndulators

PeakBrilliance

Coherent Radiation

Pulse length:tens of femtosecond

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X- FEL Science

The investigation of structural changes on ultra short time scales will become possible, thuscomplementing femtochemistry with optical lasers.

Investigation of molecular structures without the need of crystallization. This will give access to a vast number of biomolecules yet impossible to crystallize.

A new, and may be most important domain will be the non-linear interaction of X-rays and matter, leading, e.g., to multiphoton processes in atoms and moleculeswhich can not be studied with the present radiation sources.

And last not least, by focusing the X-rays to µm2 and below, one will generate plasmas at stilltotally unexplored temperatures and pressures.

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X- FEL Science

"Can we see the electron dynamics in the bonds?“"Can we see how matter forms and changes?",

"Can we take pictures of single molecules?“"Can we make a movie of a chemical reaction?“"Can we study the vacuum decay in a high field?

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X- FEL Science: Structure and dynamics of molecules

The investigation of the structure and dynamics of molecules and clusters by the diffraction of intense, femtosecond X-ray pulses. Ideally, a single X-ray pulse would suffice to record a diffraction pattern

Diffraction peaks of 21x21x21 gold atomsFrom a single X-ray pulse

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X- FEL Science: Phase transition and melting of molecules

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FEL Projects 20 today: 15 + 5 planned

Brookhaven

Argonne

DESY

StanfordJapan

0.1nm projects

Under C

ons tru ctio n

Two Projects in Italy: FERMI @ ELETTRASPARX@ Frascati

Two main projects under development: LCLS at Stanford

TESLA X-FEL at Hamburg (HASYLAB)

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LINAC Coherent Light Source (LCLS)

The Linac Coherent Light Source (LCLS) will be the world's first x-ray freeelectron laser when it becomes operational in 2009.

Electron energy 4.3 – 13.6 GeVElectron Current 1.9 – 3.4 KABunch duration: 137 – 73 fsFundamental energy: 0.83 – 8.3 KeVPeak photon flux: 31 – 5.8 1024 photon/sPeak brightness: 0.28 - 15 1032

Average brightness: 0.16 – 4.5 1022

Photon energy spread: 0.19 – 0.07 %

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LCLS Brilliance

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LCLS Beamlines and Science

Under development: two experimental hall4 exit

Coherent scattering at the nanoscale (XPCS)Atomic, Molecular, and Optical SciencePump/probe diffraction dynamicsPump/probe high-energy-density (HED) scienceNano-particle and single-molecule (non-periodic) imaging

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TESLA-XFEL

Total length: approx. 3.4 km 10 experimental stations at 5 beamlinesWavelength of X-ray radiation: 6 to 0.085 nmcorresponding to electron energies of 10-20(GeV) Length of radiation pulses: below 100 fs

Total costs of the XFEL project: 908 Meuro

Possible expansion: Second experimental hall with an additional 10 experimental stations

TESLA test facility with first SASE-FEL (TTF)The TESLA test facility TTF at DESY in Hamburg has impressively demonstrated

that the innovative technology of the X-ray laser works. From 1992 to 2004, an international team of researchers developed and tested various technical

components at this facility and thus laid the technological foundation stone for both the proposed International Linear Collider ILC (formerly TESLA linear collider)

for particle physics and for the X-ray laser project. The superconducting TESLA accelerator technology forms the basis for both

projects

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TTF Actual Status (DESY)

The Desy free-electron laser VUV-FEL is the worldwide first and until 2009 the only source of intense laser radiation in the ultraviolet and the soft X-rayrange. The 300-meter-long facility at DESY generated laser flashes with a wavelengthof 32 nanometers for the first time in January 2005 – this is the shortestwavelength ever achieved with a free-electron laser. It works as an user facility in August 2005Four experimental stations are currently available, at which differentinstruments can be operated alternately.Science applications: cluster physics, solid state physics, plasma research and biology

Actual TTF-DESY best performance:saturation at 13nmpulse length 50 fs

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FERMI

FERMI@Elettra is a single-pass FEL user-facility covering the wavelength range from 100 nm (12 eV) to 10 nm (124 eV), located next to the third-generation synchrotron radiation facility ELETTRA in Trieste, Italy.

Advanced Photo-lithography

Very high resolution and time resolved VUV and soft X-rayinelastic scattering experiments

Nano-scale spectromicroscopy

Time resolved photoemissionexperiments of molecules and clusters in the gas phase

Non-linear optical experiments in the VUV soft X-ray range

The project will make use of the existing 1.2 GeVThe facility will have two undulator chains: FEL-1: 100 to 40 nmFEL-2: 40 to 10 nmEach FEL will feed multiple experimental stations.

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FERMI-Buildings

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FERMI-Scheme

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FERMI-Time schedule

FERMI is a Single Pass FEL User Facility– 2001 Italian Ministry of Education Universities and Research announced a call forproposals for a: “Multipurpose, pulsed laser X-ray source”– 2002 Sincrotrone Trieste (Elettra) together with INFM and other Italian institutesanswered the call with FERMI@Elettra: 100 to 1.2 nm– 2004 The Project was approved & budgeted for the 100-10 nm range.– 2005 Technical Optimisation Study initiated

• Completion of the technical design study - early 2006• Linac completely free for FERMI summer 2007 (Booster commissioned)• FEL 1 “Commissioned” summer 2008• FEL 2 “Commissioned” end 2009

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SPARC - SPARX

Project SPARC of ENEA – INFN – CNR develop source, linac and undulator toward an X-ray source

SPARX1 – FEL source in the 100 – 10 nm rangein the Tor Vergata Campus

Partially funded

SPARX2 – FEL source in the 10 – 1 nm rangein the Tor Vergata Campus

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SR Applications

Micro-litography X-ray Diffraction Microtomography

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SR Experimental Methods

AbsorptionSpectroscopic methods Photoemission

Scattering

Decay processesFluorescence

(Auger) Electron emission…………………

Small spot size 0.01µ2 – 10 µ2 micro towards nanoWide spectral range: IR – Hard X-rayTime structure: 1ns – 1µs repetition rate (0.1ps length)Coherence

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Photoemission, absorption, fluorescence

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Elastic, inelastic and resonant Scattering

ω1 = ω2 Elastic scattering Diffraction

ω1 = ω2 ± ω (Internal excitation energy) Inelastic scattering

ω1 = ω2 = ω Internal excitation energy Resonant scattering

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SR Experimental Methods: Extreme conditions

Schematic of the earths crust and indication of several temperatures and pressure estimates.For a better understanding of the processes in the earthinterior one has to determine the equation-of state by experiments, because no direct access is possible.This means one needs to measure the p-V-T phase diagram for all relevant materials. Up to now only the outer part ( 2900 km below surface) is understood in detail.

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Magnetism

Origin of the magnetic moment

ferroMagnetic moments coupling

antiferrodirect exchange SuperexchangeDouble exchange……………….

3d 3dLigand 2p

Magnetic ordering (magnetic diffraction)Origin and coupling of the magnetic moments (dichroism)

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de Bergevin e Brunel sul NiO(1972)

•NiO e’ un cristallo cubico antiferromagnetico (TNeel=250 0C)•Gli ioni Ni++ hanno due soli spin accoppiati•Gli spin sono allineati magneticamente nel piano (111)•Ed antiferromagneticamente tra i piani (111)

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Surface and Interface Science

Surface diffractionGrazing incidence small-angle X-ray scattering (GIDSAX)X-ray standing wave (XSW)

Photoemission

X-ray photoelectron spectroscopy

Electronic properties of matter

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Surface Diffraction

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Total Reflection

The beam penetrates only for few nm

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Intermixing in Ge dots on Si. F. Boscherini et al. Appl. Phys. Lett. 76 (2000), 682

Si substrate

Ge dotsHeight 60 nm

Base 50-500 nmProblem: evidence the Ge-Si intermixingat the substrate-dot interface.

Samples: Grown by CVD on Si(001).

Method: XAS at the Ge K edge.

Experiment performed on GILDA with Ge EXAFS

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Interdiffusion of Ge in Ge dots on Silicon

Ge concentration and atomic ordering map showing the

location of ordered domainsinside islands

Size of islands anddomains as a function of

lattice parameter andheight.

Measured

Simulated intensity maps in the vicinity

of the Si (200) reflection.

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Photoemission: space and time resolved

Electron energySpectroscopy

Time resolvedPhotoemission

SpaceResolved

Spectroscopy

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Understanding hydrogen-metal interactions has large technological interest (i.e.: hydrogen production, storage and

burning in fuel cells)

Bulk

∆ Clean Surface∆2∆

Photoemission: an example

Chemisorption of H on Rh(100) surface at SuperESCA beamline (ELETTRA-Trieste)

Model: additivity of the core level energy shift:

hollow-bonded j=4

∆Ei,j = α i/ji= number of adsorbed atoms bondedj= adsorbate coordination number

i=1, j=4, ∆=α/4

i=2, j=4, 2∆=α/2

i=1, j=2, 2∆=α/2

Mod

el S

urfa

cebridge

bonded j=2

3∆3∆

∆∆

no 3∆ shift observed!

Forbidden configurations

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Macromolecular CrystallographyStudy and structure determination of biological macromolecules.

"The ultimate goal of molecular biology is to understand biological processes in terms of the chemistry and physics of the macromolecules that participate in them. One of the essential differences between the chemistry of living systems and that of the non-living is the great structural complexity of biological macromolecules. We shall not unravel the chemistry of life without knowing at atomic or close to atomic resolution the structure of biological macromolecules, especially the proteins.“Preface, Introduction to Protein Structure, C. Branden & John Tooze, Garland Publishing Inc., 1991.

Diffraction is the technique to study

the molecular structure of biological

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Laue pattern of a crystal of metabolic enzyme iso-citrate deydrogenase

NSLS Brookhaven

Time resolved crystallography: Exposure time: 10 ms

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Time resolved studies

Myoglobin molecule

Film of molecular processA CO molecule during interaction with a

myoglobin molecule

Fe siteCO molecule

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High Resolution and Resonance ScatteringStudy of lattice, electronic and magnetic properties in a large

variety of materialsExtreme conditions such as high pressure, low/high temperature, external magnetic field, and confined geometries.

Structural dynamics: Inelastic X-ray and nuclear inelastic scattering allow one to determine phonon dispersion relations and (partial) phonon density of states, respectively, with an energy resolution down to 0.5 meV.

Electronic and magnetic properties can be studied utilizing nuclear resonant scattering, X-ray absorption and X-ray emission spectroscopies. The corresponding dynamics can be studied by nuclear resonant scattering in the nanosecond to microsecond time regime.

Nuclear resonant scattering achieves neV energy resolution, and aims at the study of diffusion and rotational motions directly in the time domain.

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High Resolution Inelastic Scattering

!!!10EE 7−≈

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High Resolution Inelastic Scattering

Neutron: difficult to apply to disordered systems with vs>1500m/X-Rays: No kinematic limitations

no incoherent contributionssmall spot size

Neutron X-rays

θ⎟⎟⎠

⎞⎜⎜⎝

⎛ ∆−−⎟⎟

⎞⎜⎜⎝

⎛ ∆−+=⎟⎟

⎞⎜⎜⎝

⎛cos

EE12

EE11

kQ

2/1

oo

2

i 2sin2

kQ

i

θ=⎟⎟

⎞⎜⎜⎝

No cinematic limitationsThe ratio between the

exchanged momentum and the incident photon momentum

is completely determined by the scattering angle

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ESRF High Resolution Inelastic Scattering beamline

Si(7,7,7) 13.840eV 5,3meV 3.8 10-7

Si(9,9,9) 17.794eV 2,2meV 1.2 10-7

Si(11,11,11) 21.747 0,83meV 4.7 10-8

Si(13,13,13) 25.704eV 0,54meV 1.9 10-8

710EE −≤

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ESRF ID16 Analyzer

Since it is not possible to elastically bend a crystal without introducing important elastic deformations, which in turn deteriorate the intrinsic energy resolution, one has to position small, unperturbed crystals onto a spherical substrate with a radius, fulfilling the Rowland condition. This polygonal approximation to the spherical shape yields the intrinsic energy resolution, provided the individual crystals are unperturbed and the geometrical contribution of the cube size to the energy resolution is negligible.The solution realised at the ESRF consists of gluing 12000 small crystals of 0.6x0.6x3 mm3 size onto a spherical silicon substrate

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Spectroscopy with micro-nano resolution

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Focusing techniques: zone plate

λnn rrf ∆

=2

λnfrn =

22.1Re=

∆ nrsolutionSpatial

Best way to focus soft X-ray

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Focusing techniques: actual best performance in hard X-ray

[W/B4C]25 graded multilayer in vertical reflection

24KeV

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Soft X-ray microscope

Resolution: 10 nm

Field of view: 20 µm

sub-ns temporal resolution utilizing the pulsedtime structure of the storage ring in a stroboscopic

pump-probe scheme

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Synchrotron radiation based X-rayimaging and nanofocusing techniques

are promising for two reasons

first they are being applied to anincreasingly large number of subjects

including palaeontology and environmental sciences

Second, the evolution of these techniquestowards quantitative measurements with

high spatial and temporal resolutionopens new prospects in research

including the flourishing area of nano-technologies.

Scanning electron microscope image of "trichomes" from the plant Arabidopsis

thaliana. (b) Fluorescence image showing the cadmium content. (c) Fluorescence image

showing the calcium content.

Imaging techniques

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Micro-XANES Imaging

Fe distribution and oxidation state from XANES on Extraterrestrial

Grains Trapped in an Aerogel

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Soft X-ray microscope:applications

Magnetic domain pattern in a 50 nmthick (Co83Cr17)87Pt13 nanogranular alloyfilm recorded at the Co L3 absorptionedge (777eV) in an external magneticfield of 0 Oe

ContrastXMCD

Tubulin Network in Epithelial Cell

ContrastC absorption edge in the water window

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Soft X-ray microscope:Malaria infection

Blood cell infected by Malaria virus

Recentlyinfected After 36 hoursUninfected

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Coronary AngiographyFundamental concerns are associated with conventional angiography, which

requires the injection of a contrast agent directely into the coronary arteries by the mean of arterial cathetherization. The potential risks of patient mortality

and morbidity, the discomfort and the frequent hospitalization required prevent its use for routine screening or research.

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K-edge subtraction imaging

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Coronary AngiographyContrast with Iodine; in the future with Gd

The synchrotron provides a good way to assess the status of known stenoses with a less invasive method compared to conventional coronary angiography. Since the method uses venous catethers, the coronary arteries are not artificially pressurized. The resulting images are therefore in a true physiological state.The virtual absence of complications with this method allows it to by used for protocols where conventional angiography may not be allowed.

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Phase Contrast Imaging

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Phase Contrast Imaging

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Mammography

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Diffraction enhanced imaging (DEI)

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Functional Lung Imaging

Non-invasive means of quantitatively measuring regional lung ventilation.

A respiration-gated computed tomography technique (SRCT) that uses a synchrotron x-ray source. This technique allows both to image and to quantitatively measure regional lung ventilation based on the dynamics of stable Xe gas wash-in or wash-out.

One advantage of SRCT over CT techniques using standard X-ray sources, is that it allows both to visualize stable Xenon gas used as a tracer, and to directly quantify it's absolute concentration on any given point of a lung CT image.

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Functional Lung Imaging

Sequential KES tomograms in rabbit. The actual size of the image field is 98 mm × 63 mm per frame. Xenon in the airways is visible at the second image and is enhanced throughout the sequence. The heart and blood vessels appear as lucencies. The strong contrast due to the ribs is seen as an artifact in the reconstructed images. The round opacities in the right side of each image re due to the gas inlet tube.

Sequential KES chest images in rabbit. Imaging time: 0.28 s per frame, image-to-image delay: 1.3 s. The bronchial tree is visible on frames 2 and 3, down to the fourth bifurcation of approximately 1 mm in diameter

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synchrotron XRPD at GILDA (ESRF)capillary geometry transalating imaging-plate systemtime-resolved powder diffraction +Rietveld: great tool for dynamic effects

Synchrotron

radiation

Slits

IP Traslation

IP

DIGITIZED FROM TIP

EXCTRACTION USING SCANZERO

TIMETIME--RESOLVED RESOLVED ININ--SITUSITU POWDER DIFFRACTIONPOWDER DIFFRACTION

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TIMETIME--RESOLVED RESOLVED ININ--SITUSITU POWDER DIFFRACTIONPOWDER DIFFRACTION

Beam

SlitsSample

Sampleheater

Image Plateholder

The apparatus is ideal for collecting medium to relativelyhigh-resolution diffraction data from weakly scattering

samples and to investigate in-situ phase changes induced bytemperature

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Grain Nucleation and Growth during SolidificationIn the industrial production process of aluminium alloys the addition of TiB2 particles along with solute titanium is widely used to enhance the nucleation rate and control the grain growth during solidification.Although the mechanisms responsible for grain refinement were studied extensively during the last few decades, a comprehensive understanding is still lacking due to experimental difficulties in monitoring the grain nucleation and growth in situ. A question of particular interest is how added TiB2 particles along with solute titanium results in grain refinement, while no grain refinement is observed if one of the two is missing.

Time resolved diffractionAl alloy with 0.1% Ti and 0.1% of TiB2

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Grain Nucleation and Growth during Solidification

Total number of nucleated grainsand the corresponding solid phase

fraction as a function of time.

Grain radius of an individual aluminiumgrain and an individual TiAl3 grain as a function of temperature during the same

solidification experiment.