3D P

hase

Con

tras

t Im

agin

g

P. C

loet

ensa

J.P. G

uiga

ya , O

.Hig

nette

a , W

. Lud

wig

b ,R

. Mok

soa ,

M. S

chle

nker

can

d S.

Zab

lera

a ES

RF, G

reno

ble

b G

EMPP

M, I

NSA

Lyo

n, F

ranc

ec

CN

RS, G

reno

ble,

Fra

nce

cloe

tens

@es

rf.fr

1 m

m

From

arte

fact

sto

3D p

hase

con

trast

imag

ing

Unp

olis

hed

bery

llium

win

dow

Ren

derin

g of

a se

mi-s

olid

100

mµ

poro

sity

surf

ace

obse

rved

durin

g fa

tigue

‘fin

gers

’

Tom

ogra

phy

Mot

ivat

ion

3D m

icro

scop

y (n

on-d

estru

ctiv

e)in

-situ

exp

erim

ents

(stra

in, f

atig

ue, …

)‘r

epre

sent

ativ

e el

emen

tary

vol

ume’

inpu

t for

cal

cula

tions

: µst

ruct

ure

↔pr

oper

ties

Com

prom

ise

spat

ial r

esol

utio

n⇔

field

of v

iew

mic

ron

(100

nm

)m

illim

eter

, cen

timet

er

Use

r Fac

ility

Nee

d fo

r pra

ctic

al, r

obus

tmet

hods

Out

line

Abs

orpt

ion

tom

ogra

phy

Phas

e co

ntra

st to

mog

raph

y ed

ge-d

etec

tion

Hol

o-to

mog

raph

y ph

ase

retri

eval

with

imag

es a

t diff

eren

t dis

tanc

es

Para

llel b

eam

imag

ing

Futu

re n

eeds

Sour

ce: m

ore

brill

ianc

e, m

ore

cohe

renc

e?O

ptic

s: m

irror

figu

ring

Det

ecto

rs: s

peed

and

eff

icie

ncy

Met

hods

: uni

vers

al p

hase

retri

eval

Div

erge

nt b

eam

imag

ing

PCI w

ith X

-ray

mag

nific

atio

nFl

uore

scen

ce im

agin

g

Para

llel b

eam

imag

ing

•Fre

snel

diff

ract

ion

over

a d

ista

nce

D(f

ew m

m to

met

ers)

•In-

line

Gab

or h

olog

raph

y•D

efoc

usin

g in

ele

ctro

n m

icro

scop

yA

tom

reso

lved

EM

(Van

Dyc

k, E

MAT

, Ant

wer

p)

mon

ochr

omat

orsa

mpl

ede

tect

or

AB

SOR

PTIO

NA

BSO

RPT

ION

+

PHA

SE

D

plan

e m

onoc

hrom

atic

w

ave

whi

te b

eam

fr

om sy

nchr

otro

n

Para

llel b

eam

imag

ing

trans

latio

nst

age

rota

tion

stag

e

ESR

Fca

mer

a

sam

ple

Impl

emen

ted

on ID

19 /

ESR

FD

edic

ated

mic

roto

mog

raph

(P. B

erna

rd)

Mon

ochr

omat

or:

doub

le S

i cry

stal

(∆λ/

λ=10

-4)

or m

ultil

ayer

(∆λ/

λ=10

-2)

Sam

ple

stag

ero

tatio

n st

age

(tom

ogra

phy)

Det

ecto

r CC

D-b

ased

(FR

eLoN

)on

tran

slat

ion

(pro

paga

tion)

cruc

ial f

or sp

atia

l res

olut

ion

Scan

tim

e 1024

2*

900

proj

.: 7

min

utes

2048

2*

1500

pro

j.: 2

0 m

inut

es

Abs

orpt

ion

Tom

ogra

phy

Hig

h flu

x, m

onoc

hrom

atic

bea

m y

ield

s:H

igh

spat

ial r

esol

utio

nap

prox

. 1 µ

m10

243

volu

me

in 1

5 m

inut

esQ

uant

itativ

e re

cons

truct

ion

of li

near

abs

orpt

ion

coef

ficie

nt µ

(x,y

,z)co

mpo

sitio

n (b

one,

teet

h, …

)D

ynam

ic v

isua

lisat

ion

Para

llel b

eam

acqu

isiti

on se

tup

Sync

hrot

ron

sour

ceSa

mpl

e

Mon

ochr

omat

ic

X-ra

ybe

am2D

D

etec

tor

Sam

ple

stag

e

Spat

ial C

oher

ence

Wav

eis

par

tially

coh

eren

twhe

n th

e so

urce

is sm

alla

nd fa

r

Tran

sver

se c

oher

ence

leng

thso

urce

obje

ctde

tect

or

sα

blur

ring

= z 2

.α=

z 2/z

1.s

z 1z 2

szl

2.2

1co

hλ

αλ=

=

}2λ

beam

1

beam

2

θ

t coh

lα

≈0.

2 µr

ad

l coh=

λ/ 2

α≈

250

µman

dho

rizon

tally

< 1

µra

d

sour

ce

ESR

F, ID

19 B

eam

line:

L=

145

ms v

≈25

µm

s h≈

125

µm

Spat

ial c

oher

ence

•In

prin

cipl

e: c

ompl

ete

obje

ctco

ntrib

utes

to a

poi

nt o

f the

imag

eIn

pra

ctic

e: o

nly

finite

regi

on: f

irst F

resn

el z

one

radi

us

D

Dr

λ=

F

Edge

Enh

ance

men

t

Esse

ntia

lly e

dge

enha

ncem

ent

Wea

k de

focu

sing

(and

wea

k co

ntra

st!)

Rad

iogr

aphy

(2D

)

Tom

ogra

phy

(3D

)

Det

ectio

n of

crac

ksho

les

rein

forc

ing

fibre

s, pa

rticl

es

∆−

≈)

,(

21

.

)

,(

),

(0

yx

Dy

xI

yx

Ixy

Dϕ

πλ

abso

rptio

n im

age

phas

e te

rm2D

Lap

laci

an p

hase

o(x,

y,z)

≈

µ

(x,y

,z)

−

D

∆xy

zδ(x

,y,z

)

abso

rptio

n te

rmph

ase

term

Lapl

acia

n re

frac

tive

inde

x

aD

<<λ

Phas

e C

ontra

st: L

iqui

d Fo

ams

Scie

ntifi

cC

ase:

Evol

utio

n (c

oars

enin

g, d

rain

age)

of l

iqui

dfo

ams i

n 3D

F. G

rane

r (U

JF),

J. La

mbe

rt, P

. Clo

eten

s

Liqu

id

X-r

ays

Phas

e C

ontra

st: L

iqui

d Fo

ams

Scie

ntifi

cC

ase:

Evol

utio

n (c

oars

enin

g, d

rain

age)

of l

iqui

d fo

ams i

n 3D

F. G

rane

r (U

JF),

P. C

loet

ens

E =

15 k

eV, S

ampl

e-de

tect

or d

ista

nce:

0.1

5 m

1 m

m

Phas

e en

hanc

emen

t to

visu

alis

e liq

uid

film

s sep

arat

ing

bubb

les:

Film

thic

knes

s <<

voxe

l siz

eth

in fi

lms

Phas

e C

ontra

st: L

iqui

d Fo

ams

F. G

rane

r (U

JF),

J. La

mbe

rt, P

. Clo

eten

s

Coa

rsen

ing:

pre

ssur

e dr

iven

gro

wth

or d

isap

pear

ance

of b

ubbl

es

⇒3D

Gro

wth

Law

volu

me

indi

vidu

al b

ubbl

es in

tim

e(c

fr. g

rain

gro

wth

, sin

terin

g)

Qui

ckTi

me™

and

a S

oren

son

Vid

eo 3

dec

ompr

esso

r are

nee

ded

to se

e th

is p

ictu

re.

time

size av

erag

esi

ze

2 m

inut

es/s

can

(2G

B d

ata)

Hol

otom

ogra

phy

3D d

istri

butio

n of

δor

the

elec

tron-

dens

ityim

prov

edre

solu

tion

stra

ight

forw

ard

inte

rpre

tatio

npr

oces

sing

2) to

mog

raph

y: re

peat

edfo

r ≈10

00an

gula

r pos

ition

s

PS fo

am

1) p

hase

retri

eval

with

imag

es a

t diff

eren

t dis

tanc

es Phas

e m

apD

P.C

loet

ens e

t al.,

App

l. Ph

ys. L

ett.

75, 2

912

(199

9)

Hol

otom

ogra

phy

Qui

ckTi

me™

and

a d

ecom

pres

sor a

re n

eede

d to

see

this

pic

ture

.

13 m

m

E. P

agot

, P. C

loet

ens

Bre

ast B

iops

yØ

≈ 1

5 m

m ;

pixe

l siz

e =

7.5

µm

⇒H

uge

dist

ance

s: 0

.03,

1, 4

.3 a

nd 8

.8 m

!

Ener

gy =

25

keV

rad

Phas

e M

ap

Larg

er fi

eld

of v

iew

E. P

agot

, P. C

loet

ens

Bre

ast B

iops

yØ

≈ 1

5 m

m ;

pixe

l siz

e =

7.5

µm

2 m

m

ρLo

bula

r tis

sue

Abs

orpt

ion

Hol

otom

ogra

phy

Den

sity

Res

olut

ion

-0.0

4

-0.0

20

0.02

020

4060

80

rela

tive

δ

(*10

6 )

dist

ance

(µm

)

Abs

orpt

ion

Phas

e co

ntra

st

β-m

apδ-

map

E =

18 k

eV50

µm

0.00

5

0.00

55

0.00

6

0.00

65

0.00

7

020

4060

80

β

(*10

6 )

dist

ance

(µm

)

∆δ≈

3.5

10-8

⇒∆ρ

≈0.

05 g

/cm

315

% o

f Si

Sem

i-sol

idA

l / A

l+Si

Al

Al/S

i

∆δ L. S

alvo

(GPM

2, G

reno

ble)

Den

sity

Res

olut

ion

Hol

otom

ogra

phy

δ-m

ap

Sem

i-sol

idA

l / A

l+Si

L. S

alvo

(GPM

2, G

reno

ble)

-0.0

6

-0.0

4

-0.0

20 020

4060

8010

0

varia

tion

deδ

(.106 )

dist

ance

(µm

)

Inte

rden

tritic

liqu

id

Trap

ped

liqui

d

Res

ults

:In

terd

endr

itic

liqui

d15

(±1)

wt%

Si

Trap

ped

liqui

d 23

(±2)

wt%

Si

⇒O

ut o

f equ

ilibr

ium

solid

ifica

tion

∆δ

Div

erge

nt b

eam

imag

ing

Impr

ove

the

spat

ial r

esol

utio

n

λ<

1 Å

reso

lutio

n ≈

0.5

µmw

ith sc

intil

lato

r bas

ed d

etec

tors

X-r

ay m

agni

ficat

ion

usin

gdi

ffra

ctiv

eop

tics(

FZP)

refr

activ

e op

tics(

CR

L)re

flect

ive

optic

s(K

B)

Gab

or’s

Mic

rosc

opic

prin

cipl

e (N

atur

e, 1

948)

The

obje

ct is

illu

min

ated

with

by

an e

lect

ron

elec

tron

elec

tron

beam

bro

ught

to a

fine

focu

s…

The

obje

ct is

a sm

all d

ista

nce

behi

nd (o

r in

fron

t) of

the

poin

tfoc

us, f

ollo

wed

by

a p

hoto

grap

hic

plat

eph

otog

raph

ic p

late

phot

ogra

phic

pla

teat

a la

rge

mul

tiple

of t

his d

ista

nce…

Kirk

patri

ck-B

aez

focu

sing

slits

mirr

or 1

mirr

or 2

focu

s50 m

m< 30

0 m

m15

0 m Sour

ce si

zeM

irror

qua

lity

Diff

ract

ionso

urce

O. H

igne

tte, G

. Ros

tain

g

Focu

sing

resu

lts a

t 20.

5 ke

V O. H

igne

tte, P

. Clo

eten

s

Mea

sure

men

t:D

irect

line

scan

, no

deriv

atio

nFl

uore

scen

ce o

f Au

slit

Au

thic

hnes

s < 7

0 nm

X-r

ays

4.5

1011

116

x 90

600

x 16

0

2 10

1186

x 8

340

0 x

100

5 10

1011

8 x

109

200

x 50

Flux

(∆E/

E=10

-2)

ph/s

@ 8

0 m

ASp

ot fw

hmV

*H (n

m)

Ape

rture

V*H

(µm

)

Gai

n >

3 10

6!!

App

licat

ions

: Pro

ject

ion

Mic

rosc

opy

obje

ctz 1

z 2de

tect

or

equi

vale

nt to

D

+

Plan

e w

ave

illum

inat

ion

D=

z 1.z2

z 1+

z 2

1

21

zz

zM

+=

Mag

nific

atio

n

Lim

it ca

ses

z 1>>

z 2D

= z 2

; M=

1

z 1<<

z 2D

= z 1

; M=

z 2/z

1

Proj

ectio

n M

icro

scop

y2

µm p

itch

grat

ing

(Si)

C. D

avid

, PSI

D =

-10

mm

M =

230

D =

-20

mm

M =

115

D =

20

mm

M =

115

D =

10

mm

M =

230

focu

s

Expo

sure

tim

e =

0.4

s ! (1

6-bu

nch,

satu

ratio

n C

CD

)P.

Clo

eten

s, O

. Hig

nette

Proj

ectio

n M

icro

scop

y

Opt

ical

mic

rosc

ope

view

X ra

y m

icro

scop

e vi

ew

Cu

fiber

Gro

upof

cel

ls

25 µ

m

Cel

lula

r im

agin

gC

ance

rous

cel

lsS.

Boh

ic

Proj

ectio

n M

icro

scop

yC

ance

rous

cel

lsS.

Boh

ic

D =

50

mm

M =

45

D =

30

mm

M =

75

D =

10

mm

M =

230

E =

20.5

keV

Expo

sure

tim

e =

0.3

s ! (1

6-bu

nch)

No

X-r

ay o

ptic

s beh

ind

the

sam

ple

⇒do

se e

ffic

ient

Tow

ards

focu

s

10 µ

m

P. C

loet

ens,

W. L

udw

ig

App

licat

ions

: Flu

ores

cenc

e

K Fe

Pt

Step

= 0

.3 µ

m, 0

.9 se

c/pt

40 µ

m

P. C

loet

ens,

W. L

udw

ig,

S. B

ohic

Phas

e C

ontra

st

Can

cero

us c

ells

trea

ted

with

ant

i-can

cer d

rug

(Cis

plat

in)

App

licat

ions

: Flu

ores

cenc

eC

ance

rous

cel

ls (C

oll.

S. B

ohic

-ID

22)

K Fe

Pt Trac

es o

f Pt-b

ased

dru

g ca

n be

imag

edN

ew o

pens

in e

lem

enta

l cel

lula

r che

mis

tryA

dapt

ed le

ngth

scal

e fo

r-s

ub-c

ellu

lar s

truct

ures

(cel

l org

anel

les)

-uni

cellu

lar o

rgan

ism

s (ba

cter

ia, a

lgae

an

d fu

ngi)

Step

= 0

.5 µ

m1

sec/

pt

50 µ

m

P.C

loet

ens,

W. L

udw

ig, S

.Boh

ic

1600

pix

els

N

U. W

egst

, Max

-Pla

nck-

Inst

itute

, Stu

ttgar

t

90 µ

m80

pix

elsSo

urce

: mor

e ph

oton

s?

Incr

ease

N⇒

num

ber o

f pho

tons

Nph

otne

eded

incr

ease

s as N

4(F

lann

ery

87)

Mor

e co

here

nce?

Dis

tanc

eto

be

mos

t sen

sitiv

eto

leng

thsc

ale

a:

Dop

t=

a2 2λFo

r exa

mpl

e at

λ=

0.5Å

(25

keV

)

a=

1 µm

⇒

D=

10 m

m

a=

10 µ

m

⇒D

= 1

m

a=

40 µ

m

⇒D

= 16

m

a=

0.3

mm

⇒

D≈

1 km

sync

hrot

ron

patie

ntde

tect

or

sz 1

=2 k

mz 2

=2 k

m

D=

z 1.z2

z 1+

z 2

Opt

ics

Strin

gent

requ

irem

ents

on b

eam

line

optic

s:Po

lishe

d w

indo

ws,

Mon

ochr

omat

orsu

rfac

e, …

Dus

t!

Scra

tche

sD

ust

1 m

m

Ever

ythi

ngin

the

beam

can

act

as a

pha

se o

bjec

t Unp

olis

hed

Ber

ylliu

m

no th

ickn

ess v

aria

tions

(sur

face

)no

den

sity

fluc

tuat

ions

(vol

ume)

NO

OPT

ICS

No

Opt

ics

If so

urce

pro

vide

s spa

tiala

nd te

mpo

ral c

oher

ence

∆E/E

=10-2

or 1

0-4

Sing

le li

ne u

ndul

ator

s

NO

OPT

ICS

(sou

rce

-sam

ple

-det

ecto

r)

Spur

ious

con

tras

t rem

ains

maj

or li

mita

tion

of se

nsiti

vity

of P

CI

Impr

oved

sign

al-to

-noi

se ra

tio

Mor

e co

here

nce

and

bette

r opt

ics

Crit

ical

focu

sing

Pres

ent s

ourc

e si

ze li

mit

with

KB

:90

nm

x 5

0 nm

(Sou

rce

size

)(M

irror

qua

lity:

ion

beam

figu

ring)

Diff

ract

ion

ultim

ate

focu

s: 2

0 nm

(h) x

12

nm (v

)

Muc

h m

ore

effic

ient

: 0.

2 m

m x

1.2

mm

of a

20

mm

x 3

mm

bea

m

Hig

h R

esol

utio

n D

etec

tor

Dow

n to

0.5

µm sp

atia

l res

olut

ion

Effic

ienc

ydr

ops a

t hig

her e

nerg

ies

with

reso

lutio

n

optic

sC

CD

scin

tilla

tor

αX

-ray

sm

irror

X-r

ay→

visi

ble

light

conv

ersi

onC

ruci

alfo

r par

alle

l bea

m im

agin

g

In-s

ituto

mog

raph

y:go

al: 3

D im

ages

in ~

1 se

cond

(1 m

s /im

age)

CC

Dte

chno

logy

afte

rglo

wof

scin

tilla

tor

Alte

rnat

ives

nee

ded

to c

lass

ical

sche

me

X-r

ay →

visi

ble

light

→C

CD

Det

ecto

r for

hol

otom

ogra

phy

→us

ese

vera

l det

ecto

rs in

par

alle

lSc

intil

lato

riss

emi t

rans

para

nt

Sam

ple

CC

DC

CD

CC

DC

CD

Met

hods

: uni

vers

al p

hase

retri

eval

Cas

es th

at w

ork

wel

l:sl

owly

var

ying

pha

se (a

nd sl

ow a

bsor

ptio

n)w

eak

phas

e (a

nd w

eak

abso

rptio

n)

Gen

eral

cas

e:di

stan

ce w

ith o

ptim

um c

ontra

st c

an o

ften

not b

e us

edlim

itatio

n to

smal

ler d

ista

nces

due

to a

lgor

ithm

s

Poor

sens

itivi

tyto

low

spat

ial f

requ

enci

essu

ppor

thel

ps, b

ut m

etho

d be

com

esite

rativ

e

Met

hods

: uni

vers

al p

hase

retri

eval

Com

bina

tion

with

‘diff

ract

ion’

imag

ing

(cf.

Fien

up)

not l

imite

d to

smal

l obj

ects

supp

ort g

iven

by

edge

enh

ance

men

t‘lo

w’ r

esol

utio

n im

age

from

near

and

inte

rmed

iate

fiel

dhi

gh sp

atia

l fre

quen

cies

from

wea

k no

n-lin

ear i

nter

fere

nce

term

sD

obje

ct p

lane

imag

e pl

anes

Ove

rsam

plin

g in

real

spac

e

Des

troyi

ng th

e in

terf

eren

ce p

atte

rn

Spin

ning

inho

mog

eneo

us m

ater

ial:

woo

d, ..

.

App

licat

ions

: ho

mog

eneo

usbe

amin

cohe

rent

illu

min

atio

nin

X-r

ay m

icro

scop

y

Alte

rnat

ive

Ran

dom

hol

ogra

phic

gra

ting

(O. H

igne

tte)

Chr

. Dav

id (P

SI -

CH

)

nylo

nfib

re

100

µm

rand

om g

ratin

g

P. C

loet

ens,

T. B

igau

lt(E

SRF)

Con

clus

ions

Cha

roph

yte

foss

ilsS.

Zab

ler

•Im

prov

emen

ts in

bril

lianc

e ar

e im

porta

ntbu

t als

o op

tics,

dete

ctor

s and

met

hods

•Tom

ogra

phy

mor

e po

wer

ful t

han

ever

: abs

orpt

ion,

pha

se c

ontra

st,

holo

tom

ogra

phy,

…•Q

uant

itativ

em

appi

ng in

2D

and

3D

•Pro

ject

ion

mic

rosc

opy

by K

B fo

cusi

ng:

(90

nm)2

focu

sing

mad

e ‘e

asy’

Hig

h flu

x (1

012ph

/s)

Mic

ro-s

truct

ure:

fast

nan

o-ra

diog

raph

y, n

ano-

tom

ogra

phy

Fluo

resc

ence

: for

sub-

mic

ron

elem

ent m

appi

ng (2

D -

3D)

Ack

now

ledg

men

ts•

GPM

2, IN

PG, G

reno

ble

L. S

alvo

, Ch.

Joss

eron

dSe

mi-s

olid

s•

Spec

trom

etrie

Phy

siqu

e, G

reno

ble

F. G

rane

rU

niv.

Not

re D

ame,

Indi

ana

J. G

lazi

erG

MC

M, U

niv.

Ren

nes

J. La

mbe

rt, R

. Del

anna

yLi

quid

Foa

ms

•ES

RF

supp

ort g

roup

sG

. Ros

tain

g, P

. Ber

nard

, Chr

. Mor

awe

D. F

erna

ndez

, A. M

irone

•EM

AT,

Uni

vers

ity o

f Ant

wer

pD

. Van

Dyc

kPh

ase

Ret

rieva

l•

ID19

Bea

mlin

e ES

RF

E. B

olle

r, X

. Thi

baul

t, J.

Bar

uche

l•

Med

ical

Bea

mlin

e ES

RF

S. F

iedl

er, A

. Bra

vin

brea

st im

agin

g