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