nx12 imaging i - oak ridge national laboratory14th national school on neutron and x-ray scattering...

X-ray Imaging

Ian McNultyCenter for Nanoscale Materials

16 August 2012

14th National School on Neutronand X-ray Scattering

Argonne National Laboratory

I. McNulty NX2012 16 August 2012

Outline

Part I 1. Fundamentals

resolutioncontrastx-ray sourcesx-ray optics

2. Direct methodsprojectionfull-fieldscanning

Part II 3. Indirect methods

microdiffractioncoherent diffractionholography


1. Fundamentals

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! )$(*+,#*

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References: 1. M. Howells, "Soft-x-ray microscopes," Physics Today 38, 22 (Aug. 1985). 2. J. Kirz and H. Rarback, "Soft xray microscopes," Rev. Sci. Instrum. 56, 1 (1985). 3. J. Als-Nielsen and D. McMorrow, Elements of Modern X-ray Physics (Wiley, New York, 2000). 4. D. Attwood, Soft X-Rays and Extreme Ultraviolet Radiation: Principles and Applications (Cambridge, 2007). 5. J. Goodman, Introduction to Fourier Optics, 3rd ed. (Roberts and Company, 2005).


Imaging

image [ˈɪmɪdʒ]

Noun:The optical counterpart of anobject produced by an opticaldevice (as a lens or mirror) oran electronic device

Verb:Make a visual representation of(something) by scanning it witha detector or electromagneticbeam.

- Merriam-Webster Dictionary


Image formation as a scattering process

Incident waves with initialmomentum kinc are elasticallyscattered into new direction kscattwith momentum transfer !k.

Ewald sphere is defined by conservation of momentum. Only spatial frequencies onthe Ewald sphere are accessible to the imaging process, limiting attainable resolution.

kscatt

kinc

!k"

kscatt

k inc

Ewaldcircle

object spatialfrequency limit

kz

ky

!

k

kx

kzk inc

kscatt


!

P(x,y) =sin xx

sin yy

!

"k = kinc # kscatt

!

kx2 + ky

2 + (kz + kinc)2 = kinc

2

!

(0 " #k " 2kinc)

!

(kz << kinc)!

kx =2"2R

=2"#NA

!

kz =kx2

2kinc

!

x =kaxz

!

y =kayz

Point-spread function

For extreme-angle ray (xz plane, ky = 0) with

Transverse

Longitudinal

!

NA ~ az

!

k =2"#

where

with ,

Bragg's law

and

P(x)

kax/z

" 1.0R

!

DOF ="

(NA)2

!

R = 0.5 "NA

Diffraction limits to resolution

x

y

z

a

P(x,y)


What do we mean by "resolution"?


!

P(x,y) =sin xx

sin yy

!

"k = kinc # kscatt

!

kx2 + ky

2 + (kz + kinc)2 = kinc

2

!

(0 " #k " 2kinc)

!

(kz << kinc)!

kx =2"2R

=2"#NA

!

kz =kx2

2kinc

!

x =kaxz

!

y =kayz

Point-spread function

For extreme-angle ray (xz plane, ky = 0) with

Transverse

Longitudinal

!

NA ~ az

!

k =2"#

where

with ,

Bragg's law

and

P(x)

kax/z

" 1.0R

!

DOF ="

(NA)2

!

R = 0.5 "NA

Diffraction limits to resolution

x

y

z

a

P(x,y)


longitudinal coherence

#!#

!

d " # = $ /2%

!

"x "p # h /2

Coherence

!

lc ~ "2

#"

!

"c ~ #2

c$#

!

w c ~ "zd

transverse coherence

d2$

!

wc


Coherent vs. incoherent

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X-ray microscopy: early history

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! 1946 - 1971: Engstrom developsquantitative elemental imaging,Kirkpatrick and Baez developcrossed-mirror system for focusing x-rays, Cosslett and Nixon developpoint-projection microscopy methods.Baez suggests use of zone platelenses.


useful complement to


X-ray microscopy: early history

! 1972 - 1993: Horowitz & Howellbuild first scanning microscope atCambridge Electron Accelerator,Aoki and Kikuta perform x-rayholography experiments, Schmahlbuilds first transmission x-raymicroscope at DESY and ACO,Rarback & Kirz advance scanningmicroscopy with zone plates atNSLS. Schmahl & Rudolphdevelop Zernike phase contrastmicroscopy.


X-ray microscopy: recent history

! 1994 - 2002: Scanning andtransmission x-ray microscopesproliferate at facilities wordwideincluding ALS, ESRF, ELETTRA,NSRRC, APS, and SPring8.– 3D imaging via tomography and

cryo-tomography take off.– Coherent diffraction imaging first

demostrated by Sayre & Miao.

! 2003 - present: X-ray microscopesbecome commercially availableand that use laboratory sources.Applications expand to includeenvironmental, geological/cosmo-chemistry, polymers, biology,magnetism, materials, and energyscience, among others.


Si atoms - 0.078 nm spacing

Fe quantum corral - 14 nm

DNA - 2.5 nm

Red blood cell - 8 µm

Fly ash 10-20 µm

Mitochondria - 500 nm

Why x-ray microscopy?


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X-rays offer:


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Contrast mechanisms in x-ray imaging


!

A = A0 exp("inkt)k = 2# /$

!

n =1"# " i$ =1" re2%

&2 ni fi (0)i'

• Absorption contrast:

sensitive to Im(n)

• Phase contrast:

sensitive to Re(n)

Refractive index and contrast in the x-ray region

!

~ 2"#(x,y)t /$

!

~ 4"#(x,y)t /$


Absorption edges provide elemental and chemical specificity


Details of edge spectra tell us about chemical state


The "water window"


Fluorescence spectroscopy


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>100?00#@03

Why use synchrotron radiation?


x

p

x

p

Ac

Undulator radiation

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Focusing optics for x-rays

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Fresnel zone plate

!

f 2 + rn2 = f +

n"2

#

$ %

&

' (

2

rn2 = nf" +

n2"2

4

rn ) nf"

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Resolution of a zone plate

R


A zone plates forms an image like a thin lens

!

1s1

+1s2

=1f

!

1p

+1q

" 1f

M = pq


Efficiency of a gold zone plate


12 nm lines Si/Mo

20 nm zone plate25 nm zone plate 17 nm zone plate

10 nm lines Si/Mo20 nm (vertical) Au lines

9 nm lines Si/MoImaged by 17 nm zone plate

All images taken at 700 eVStructures have equal line/space nominal dimensionsDimensions of half periods are quotedAchieved resolution close to the theoretical limits

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Performance of best zone plates to date


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References: 1. M. Howells, "Soft-x-ray microscopes," Physics Today 38, 22 (Aug. 1985). 2. J. Kirz, "Soft X-ray microscopes and their biological applications," Q. Rev. Biophys. 28, 1 (1995).

2. Direct methods


Direct imaging methods

Scanning

Full-field

Projection


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X-ray beam

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Different regimes for x-ray imaging


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a ba b

Phase contrast: tool of choice for low absorption samples


150 ps

472 ns

1.59 us

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150 ps

17 ns long each, 220 ns apart

1.59 us

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Utilizing the time structure of the source


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High-speed imaging of jets and droplet coalescence


Full-field x-ray microscope

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XM-1 microscope at the ALS


Wet specimens can be studied up to damage limits

Whole, hydrated mouse epithelial cell


Cryo-preparation of sample mitigates radiation damage


Interconnects in chips are more "hardy"


Binary Alloy

Dealloying: selectively dissolvethe less noble component in acid

NanoporousMetal

Nanoporous Aufrom AgAu

200nm

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Another example: nanoporous metals

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How does the dealloying process proceed?


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22 µm

Following coarsening during annealing at 600°C


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Interfacial surface distribution indicates coarsening doesnot proceed by bulk diffusion


Polarized x-rays give sensitivity to electron spin


Magnetic x-ray microscopy

Magnetic recording materials:FeTbCo multilayer with Al cap layer

P. Fischer et al. (LBL)


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Spin current induced domain wall motion


Differential interference contrast (DIC)

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"XOR" DIC

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3D imaging

R ! 0.61 # / NA DOF ! 1.22 # / (NA)2 = 2 R2 / (0.61#)

|n| ! 1 ) NA << 1 ) DOF << R

Synthesize larger NA with multiple views

Cannot improve R, only DOF by tomography

! t

! l

RDOF


Computed tomography

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Invert S I(x, y,!){ } " µ(x, y, z)

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X-ray nanotomography of cryo-preserved yeast


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Gordon Research Conference March 4-9, 2012

Designing stable electodes for Li battery cells

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Quantitative phase tomography


Full-field microscopy with hard x-rays


Scanning x-ray microscope

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Detect both fluorescence and transmitted signal inscanning mode


APS 2-ID-E scanning x-ray microscope


Example: Ta-lined Cu interconnect, W vias

10 µm

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0º

30º

Use to probe buried defects in microelectronic devices


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Study light elements with 1-4 keV x-rays

2 !m

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Al P

Si sum

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[$,2%5*')10/#81$'1)'"#+"%*/'361236#5.'%$'/#0%$.'2.(%/.$52'%2'P$1<$'51';.'#'/#n10'2%$P')10'56.N%5#+'$*50%.$5'36123610*2C';*5'%$G'%5')10/2'%2'#'/425.04E'!.(%/.$5'"6./%2504'%2'$15'"1$(*"%N.'5130."%3%5#81$'1)'56.2.'/%$.0#+2E

!"#$$%$&'U,0#4'23."501,/%"012"134'261<2'(%#51/,(.0%N.('31+4361236#5.2'3+#4'#'"0%8"#+'01+.'%$'T2.Z*.250#81$E'76%2'/."6#$%2/'.U3+#%$2'56.'3*::+%$&+4';01#('(%250%;*81$'1)'56.2.'/%$.0#+21;2.0N.('<10+(<%(.E

\#0%$.'31+4361236#5.')10/#81$'%$B*.$".2'&.1+1&%"#+'T'2.Z*.281$'

DE'@%#:C'!"%.$".'d=JC'Ig='K=JJHM

X-ray spectra reveal chemical state with exquisite sensitivity


Energy (eV)704 708 712 716 720 724 728

parallelanti-parallel

M'some XMCDMagnetite XMCD

_++%38"#++4'T1+#0%:%$&'v$(*+#510

?33+.'[['_Tv#++'i'/#&$.5'#00#4&%0(.02'/1N.#;+.

-"/2

+"/2

0 R.C.P.L.C.P.

-.+,/0A$%,+9^,'$(#

^.)1"*2%$&'/%0010

\1$1"601/#510

FE'`#/C'96./E'r.1E'=kJC'GGJ'K=JGJM

R.A.D. Pattrick,Eur. J. Mineral. 14 (2002) 1095

gJJ'$/

GJJ'$/

Energy (eV)704 708 712 716 720 724 728

Optical D

ensity

0.0

0.1Left circ. pol.Right circ. pol.

magnetosome XMCDmagnetite XMCD / 2

Opt

ical d

ensity

Whole chain

One magnetosome

Magnetite Fe 2p spectracourtesy E.J. Goering - seeJ. Mag. & Mag. Mats 310(2007) e2493

GJJ'$/

Each crystalsite has adifferent XMCDsignal

Magnetosomes areFe(II)-rich relative tomineral magnetite

Bio-magnetism: magnetotactic bacteria


X-ray abs.

X-ray DPC

Complex transmission function: exp(i ' kt) exp(- ( kt) phase shift absorption

Use differential phase contrast for biological specimens


b!?!3."%/.$

_(*";+,'(;8"*"1*$+

9.$50#+2513 x1$.

3+#5.

E9;(,%'c'7b7?`

5 µm latex spheres, E = 2.5 keV

STXM: absorption contrast


9.$50#+2513 x1$.

3+#5. !3."%/.$b!?

7'z']7'{']

5 µm latex spheres, E = 2.5 keV

@T9m2%&$#+

c

)$(D;&+"88"*"1*$+

STXM: differential phase contrast

\E'(.'D1$&.C'T^`'GJJC'GIdLJ='K=JJHM


Developed for NSLS STXM: M. Feser, NIM A 565 (2006)

2nd generation optimized for APS

Charge integrating segmented Si detector:- segmentation matched to experiment- simultaneous recording of all segments- read by multichannel V/F or ADC -- 1 msec dwell typ., sub-msec achievable

Dead time ~ 10 us

Repeat rate ~ 50 us

Chip fabrication: Max Planck Semiconductor Lab, Munich

1

23

54

6

7

98

1200 µm diameter

]E'j10$;.0&.0C'T6E@E'76.2%2'K=JJkM

Charge integrating silicon DPC detectorB. Hornberger, C. Jacobsen (Stony Brook U.),

M. de Jonge, S. Vogt (ANL), D. Paterson (Australian Synchrotron)


radi

ans

Phase

Pennate diatoms

!m

Thickness

2535 eV, 30 nm steps,5 ms dwell (3 h scan)


• Catalyzes production of highly reactive oxygen species

) oxidative damage to lipids, proteins, DNA, etc

• Defects in regulatory processes may led to:$ Menkes syndrome

$ Wilson’s disease

$ Amyotropic lateral sclerosis (ALS)

$ Alzheimer’s disease

• Need to understand cellular uptake, trafficking, storage of Cu

• Novel Cu(I) fluorescent sensor (CTAP-1) was recently developed

) Does it reflect the true cellular distribution?

Mouse fibroblast cell + 150 #M CuCl2

CTAP-1 visiblefluorescence Cu XRF map

Copper is an essential trace element for all life forms


energy [keV]re

l.

ab

so

rba

nc

e8.97 8.98 8.99 9.00 9.01 9.02

0.0

0.2

0.4

0.6

0.8

8.96 8.97 8.98 8.99 9.00 9.010.0

0.5

1.0

1.5

2.0

energy [keV]

abso

rban

ce

nucleus

cytoplasm

Cu(I)Cu(II)

Standards

!-XANES indicates Cu(I) is present (reducing environment)

`E'l#$&C3T>?!'GJ=C'GGGkL'K=JJgM


Ban

glad

esh

Bro

wn

Ric

e

• Rice production increasingly occurs in Asand metal contaminated soils in Asia

• S-XRF was utilized to locate As in polished(white) and unpolished (brown) rice grainsfrom the United States, China, andBangladesh

• As dispersed in white rice but localized inthe pericarp and aleurone layer of brownrice - Cu, Fe, Mn, and Zn localizationfollowed that of As in brown rice

• µ-XANES and bulk extraction revealed thepresence of mainly inorganic As anddimethylarsinic acid.

?E'\.6#0&C'_$N%01$E'!"%E'7."6$1+E'i=C'GJgG'K=JJHM

US

Whi

te R

ice

There is worldwide concern over elevated arsenicconcentrations in contaminated rice paddies


! >#$12"#+.'"+*25.0%$&'1)'/.5#+'%/3*0%8.2'#5'%$50#&0#$*+#0'(%2+1"#81$2'%2'1;2.0N.(<%56%$'%$(*250%#+'/*+8,"0425#++%$.'!%'21+#0'".++2

! 9+*25.02'(%0."5+4'"100.+#5.'<%56'+1"#+'0."1/;%$#81$'#"8N%54'<%56%$'56.'21+#0'".++C0.&*+#8$&'%52'1N.0#++'36151,"1$N.02%1$'3.0)10/#$".

\E'].051$%C'_$.0&4'|'_$N%01$E'!"%E'iC'i=g='K=JGGM

!"1$C<9(,'$(.,1':"(%2+1"#81$2'51'"1$5#%$'#6%&6'(.&0..'1)'V.'#$(9*'(."10#81$E

!"1$C<9(,'$(.9(,1':"(%2+1"#81$2'#33.#0"+.#$E

Small defects mean big problems for solar cells


CO2

Mehta, P.K., in Sixth CANMET/ACI/JCI Conference: Fly Ash,Silica Fume, Slag & Natural Pozzolans in Concrete, 1998.

7% to 8% globally

limestone

Cement

primaryprecursor

Transportation

Electricity for operation

Fossil fuel combustion

Portland cement and CO2 emission


r.131+4/.02'#0.';.%$&'(.N.+13.(#2'#$'.$N%01$/.$5#++4';.$.-"%#+0.3+#"./.$5'51'T105+#$('"./.$5

)10'"1$"0.5.'301(*"81$

j#0('U,0#4'$#$1301;.'"+#0%-.2'56.3110+4'*$(.02511('6.5.01&.$.%54

#$('"1/3+.U'"6./%2504'1)&.131+4/.02

DE`E'T01N%2C'`#$&/*%0'=gC'GGHLk'K=JJLM

CO2

decarbonation of limestonekiln fuel combustion

distribution

Portland cement manufacture:

t,0#4'B*10.2".$".'/#32'1)'#'64(01U%(.,#"8N#5.('&.131+4/.0

K Fe

Ca Cr

V.'#$('902501$&+4"100.+#5.(

“Green” geopolymeric cement can reduce annualworldwide CO2 emission by tens of mega-tons


K?,VM'`1$&%5*(%$#+'2+%".2'261<%$&'!%K&0#4MC'V.'K10#$&.MC'\$'K0.(ME'T'K;+*.MC!'K4.++1<MC'9+'K4.++1<,&0..$MC'#$('x$K3*03+.E'KrM'70#$2N.02.'2+%".'261<%$&"4513+#2/%"'3%++#0C'N#"*1+.C'#$(#221"%#81$'1)'5<1'T,;1(%.2'<%56'3%++#0E

M. De Jonge, PNAS 107, 15676 (2010)9E'/.$.&6%$%#$#

Use fluorescence to see 3D elemental distribution


20mm

solid-angle ~1.5 steradiansDetector array

Sample

Beam

384 x Si detector array

960%2'^4#$'K9![^bM

Maia detector removes all overheads,dramatically increasing detection efficiency

Collaboration between CSIRO, BNL, AS & NSLS

• solid-angle ~1.5 str (~10*previously!)

• on-board, event-mode processing reducesoverheads to zero; GeoPIXE analysissupplies real-time analysis

Maia detector: a revolution in fluorescence imaging


1D multilayer Laue lens

Where is the limit for x-ray focusing ?

jE9E'F#$&C'T^`'LIC'G=kiJG'K=JJIM


Deposited multilayer

Sectioned graded-period multilayer

1D MLL

2D focusing with a multilayer Laue lens

2D MLL

• Deposit varied depth-graded multilayer on flatsubstrate (thinnest structures first)• Section to 5-20 !m depth• Assemble into a linear MLL• Assemble two linear MLL’s into a 2D MLL.

Material: WSi2/Si

Total depositionthickness: 13.25 um

d-spacing: 5 – 25 nm

drn = 25 nm

drn = 5 nm

varied line-spacingmultilayer

substrate

adjusttilt angle


MLLs are approaching the 10 nm limit of "thin" lenses

Photon Energy: 19.5 keV

Measured Resolution: 25 x 40 nm

Diffraction Efficiency: 17%jE'l#$C'b35E'_U30E'GLC'GgJIL'K=JGGM


Summary

1. Fundamentalsresolutioncontrastx-ray sourcesx-ray optics

2. Direct methodsprojectionfull-fieldscanning

(and lots of examples)


Problems

G O6#5'%2'56.'+1$&%5*(%$#+'"16.0.$".'+.$&56')10'#'GiEi'P.m'U,0#4';.#/'#$('}_'c'G'.m'y

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d ?':1$.'3+#5.'6#2'#'=J'$/'-$.25':1$.'<%(56'#$('GJJ'$/'(%#/.5.0E'O6#5'%2'K#M'56.')1"#+'+.$&56')10'�J'P.m'U,0#42yK;M'O6#5'%2'%5'g'P.m'U,0#42y

i ?3301U%/#5.+4'<6#5'U,0#4'.$.0&4'%2';.25'51'3.0)10/'/%"012"134'<%56'#;210381$'"1$50#25'1)'10&#$%"'/#5.0%#+'%$#$'#Z*.1*2'.$N%01$/.$5y'O6#5'.$.0&4'%2';.25'51'138/%:.'56.'36#2.'"1$50#25y'?22*/.'56.'10&#$%"'/#5.0%#+'%2'G~/'56%"P'2*001*$(.(';4'='~/'515#+'56%"P$.22'1)'<#5.0E

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k l1*'6#N.'#'I'$/'r#?2'$#$1(15C'#'GgJ'$/'?*'31+4"0425#++%$.'"+*25.0C'#$('#'='~/'0#5'3#$"0.#2'".++E'O6#5'543.'1)U,0#4'/%"012"13.'<1*+(';.';.25'51'%/#&.'.#"6y'O6%"6'<1*+(';.25';.'25*(%.('<%56'.+."501$'/%"012"134'%)'41*6#('56.'"61%".y

H @.0%N.'56.';#2%"'.U30.22%1$'(.2"0%;%$&'56.'x.0$%P.'36#2.'"1$50#25'U,0#4'/%"012"13.E

nx12 imaging i - oak ridge national laboratory14th national school on neutron and x-ray scattering...

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