Claudia_Gavrilescu_XRAY Technology.pdf

8/10/2019 Claudia_Gavrilescu_XRAY Technology.pdf

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AMS 2000-Rigaku representative Claudia Gavrilescu

Analytical Division Product Manager

DiffractionDiffractionAbsorptionAbsorptionFluorescenceFluorescenceReflectivityReflectivity


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Tokyo, Japan Rigaku Group Headquarters Rigaku Corporation

R23, 4pplication Research ab. Sales 2 Ser#ice

Berlin, GermanyRigaku European Headquarters

! Sales 2 Ser#ice

Prague, Czec Repu!lic Rigaku Inno"ati"e Tec nologies Europe

! 3etector and "ptics R23! *anufacturing

Houston, T#, $%&Rigaku &mericas Corporation

! Sales 2 Ser#ice! R23, 4pplication Research

ab.! *anufacturing

Bei'ing, C ina! R23! *anufacturing! Sales 2 Ser#ice

&u!urn Hills, (I, $%&Rigaku Inno"ati"e Tec nologies Inc)

! 4d#anced "ptics R23, 4pplication Research ab.! *anufacturing! Sales 2 Ser#ice

%an *iego, C&, $%&Rigaku &utomation Inc)

! &rystalli6ation 2 Sample+rep 4utomation! *anufacturing! Sales 2 Ser#ice

7hree factories in Japan7okyo for /R3 and 74, "saka for /RFand 8amanashi for /R3, /RFmanufacturing

%e"enoaks, +ent, England Rigaku Europe

! Sales and Ser#ice

Tucson & , $%&EIT

! &&3!R23 and manufacturing

(a'or o--ices (a'or distri!utors

Rigaku group


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Rigaku creates /0rayinstruments and componentsfor use in a di#erse #ariety ofapplications and fields,presenting scientists %ith auni ue le#el of depth andconfigurability.

Product areas

/R3 S4/S 3etectors Small*olecule

/RF /0ray:enerators"ptics

Stress 4nalysis

+rotein&rystallography

&ryogenics 4utomation Semiconductor

(&+E &CH.ICE))))


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General presentation of R igak u company


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R ange of R igak u products X - R ay d iffraction (X R D )

&--orda!le general purpose di--raction/ (ini0le1 II %orld;s smallest /R3 system

MiniflexII

&d"anced #R* instrumentation/

$ltima I2 3 TTR III multi0purpose


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R ange of R igak u products X-Ray Fluorescence (XRF)

%equential 6a"elengt dispersi"e systemsSupermini

%upermini 7he %orld=s first high0po%ered bench top %a#elength dispersi#e /RF

%# Primus3 %# Primus II fle ible ultra0high0performance

%imultaneous 6a"elengt dispersi"e systems

0 %imulti1 89 for e tremely high throughput

0%imulti1 8: *ulti0channel0type %a#elength dispersi#e system Primus II

%ingle c annel 6a"elengt dispersi"e system (ini7 series Benc top ;*#R0 analyzers /(ini7


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R ange of R igak u products Sm. Mol. Crystallography

! Benc top #7ray crystallograp y 7 %C#mini 0 the first benchtop /0ray crystallography system for automated threedimensional >)3? chemical structure determination

7 #ta4&B mini 6orld>s smallest for routine structure analysis

SCXmini

! CC* systems

0 %aturn ?9:@ is the ne t generation of &&3 camera XtaLA mini for small molecule crystallography

7 (ercury @ affordable compact design, ideal compact &&3 for small moleculecrystallography

! #7ray generators

- ultra# 8A ig 7-requency 8A k; #7ray generator designed for fle ibility, high stabilityand lo% maintenance operation


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R ange of R igak u products!otal Re"lection X-ray Spectrometry (!XRF)

T#R0 spectrometer -or material, c emical, en"ironment

05&5.H$5TER >Ainner of the @$$ R23 1$$ 4%ard for technical inno#ation?

7he system can measure the full range of samples, including bulk solids, li uids, po%ders,and thin films.

0 +erform trace le#el elemental analysis 0 +roduce results %ithout a %et lab 0 +redict thin0film chemical properties

#anohunter
http://www.rdmag.com/awards.aspxhttp://www.rdmag.com/awards.aspx


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R ange of R igak u products

X-ray A$sorption Spectroscopy (%XAFS & XA#%S)

/0ray absorption spectrometer >R0/4S? is a #ersatile in0house instrument capable ofperforming /4S, /4B-S, and -/4FS measurements.

7he # 0ray a!sorption spectrum can be di#ided into near edge and e tended finestructure.

0eatures/

Coth transmission and fluorescence measurements are possible.

&a to ' measurements capabilities for both opa ue and transparent

samples %ith little sample preparations

Dori6ontal or #ertical sample mounting.


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R ange of R igak u products

X-ray A$sorption Spectroscopy (%XAFS & XA#%S)

&pplications/

! -/4FS > E1tended #7ray a!sorption -ine structure= &oordination en#ironment Cond lengths

ocal disorder Ealence state

! /4B-S > #7ray a!sorption near7edge structure= Fermi energy

ocal coordination geometry

7he interpretation of /4B-S spectra is substantially more complicated than -/4FSspectra.


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R ange of R igak u products Semicon'uctor Metrology

! T in -ilm c aracterization process tools

7 (0( for metal film monitor 0 Integrates -3/RF 2 /RR in one tool >)$$ mm?

;a-er# D for thickness 2 composition A3/RF for high resolution 2 throughput >)$$ mm?

! Contamination process tools !XRF- **

T#R072D for in0process %afer contamination! Aorld;s first integrated E+3> vapor phase decomposition) 2 7/RF

>)$$ mm?, 1$ atoms)$$ mm? &T# %eries /R3 tool for thin films


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M ethods with A pplications inM icro and N anotechnology

7he common factor in nanotechnology is the dimension of the structures studied.

Banotechnology research and de#elopment relies on accurate measurement of atomicand molecular distances %ithin structures ranging from semiconductor de#ices to nano0po%ders.

/0ray diffraction >/R3? and associated techni ues are primary tools for thenanotechnology researcher.

/0ray reflectometry >/RR? determines layer thickness, roughness, and density foramorphous andsingle crystal?.

/0ray diffuse scattering is used to determine lateral and trans#ersal correlations,distortions, density, and porosity.


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M ethods with A pplications inM icro and N anotechnology

In0plane gra6ing incidence diffraction>:I3? is employed to study lateral correlations ofthinnest organic and inorganic layers as %ell as depth profiling and Inhomogeneities inmaterials.

Small angle /0ray scattering >S4/S? can determine the si6e, shape, distribution,orientation, and correlation of nano0particles present in solids or solutions.

Digh0resolution triple0a is /0ray diffraction pro#ides a nondestructi#e, uick, and uantitati#e measure of the film uality and possible defect density.

7otal Reflection /0ray Spectrometry >7/RF? and E+307/RF are tools for contaminationmeasurement, trace0le#el elemental analysis, pro#ide e#aluation of the physical nature ofthe sample and pro#ide chemical information as a function of analysis depth.

/0ray absorption spectroscopy>/4S? can measure the atomic #alence and coordinationstate of selected element by measuring its absorption spectrum. /4S


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T in -ilm analysis and%% applications

+Mo'ern metho's o" analy,ing thestructure o" material science


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T(


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0lat sample&1ial di"ergence%ample a!sorption%ample displacement

Cali!ration Internal


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$

@$$$

I$$$

F$$$

J$$$

1$$$$

1@$$$

)$ I$ 5$ F$@ > deg. ?

I n t e n s

i t y

> & +

$

1$$$

@$$$

)$$$

I$$$

5$$$

)$ I$ 5$ F$@ > deg. ?

I n t e n s

i t y

> & +

Sample preparation

+C


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0I$$$

0@$$$

$

@$$$

I$$$

F$$$

J$$$

1$$$$

5 1$ 15 @$ @5 )$ )5 I$ I5 5$@ > deg. ?

I n t e n s

i t y

> & + S ?

0I$$$

0@$$$

$

@$$$

I$$$

F$$$

J$$$

1$$$$

5 1$ 15 @$ @5 )$ )5 I$ I5 5$@ > deg. ?

I n t e n s

i t y

> & + S ?

+referred orientation

+acked oose$$) $$

$$9

+C


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7hin film analysis

+C

+hotocatalyst film > @$$nm ? on glass

$

@$$$

I$$$

F$$$

J$$$

1$$$$

1$ @$ )$ I$ 5$ F$

@ > deg. ?

I n

t e n s

i t y

> a . u .

?

000

deg.?


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:oniometer 2 optics


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&ross Ceam "ptics

Rigaku patented technologyCC and +C geometries are simultaneously

mounted, aligned, and selectable.

#7ray source

Focusing beam is selected. +arallel beam is selected.

(ultilayer mirror

%ample

Bragg7Brentano -ocusing geometry


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"pticsBragg7Brentano -ocusing+hase id, crystal structure, etc.

for po%ders

Parallel !eam+hase id, crystal structure, etc.

for thin films

Ge 97!ounce&rystal structure, film thickness, etc. for imperfect crystals

Hig resolution 3 triple7a1is

&rystal structure, film thickness, etc. for highly perfect crystals

In7plane geometry3epth controlled phase id, etc.

for ultra thin films


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&C" %


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Light Scattering

Small-AngleX-ray Scattering

10m 100nm 10nm 1nm 0.1nm1m

SAXS analysis deals with the size of about2nm~100nm!"a#ious mi$elles &olyme#s o# $olloids $an be ta#'ete

S A X

S

Ultra Small-AngleX-ray Scattering U

S A X S

U S A X

S

&hallenge for arge +article Si6e 3etermination

'0S4/S >'ltra S4/S?

'S4/S


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'0S4/S >'ltra S4/S?

Bonse7Hart camera


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Sealed0off and rotating anode

0ray tube! Seald0off 0ray tube! 97D k;

! Rotating anode tube! 78A k;

filament ta#'et

window

#otatin'

filament ta#'et

'S4/S

S4/S


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'0S4/S >'ltra S4/S?

*ultilayer mirror

:e>@@$?

/0ray source Slit1 Slit@Slit)

:e>@@$? 4ttenuator

3etector

Sample

H a isDeight limit slit *Custom-order geometry

'S4/S

'S4/S


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0.05 0.10-0.1 0.050

5.0x10 7

1.0x10 8

1.5x10 82.0x10

8

2.5x10 83.0x10 8

q(1/nm)

(cps)

U !"2 mm #$

Direct Beam Profile

q%0.0023 nm -1

!"10 mm #$

&'# n U !" +s q%0.0023 nm -1 (2%0.0032 deg).&'# n 2s, ts !" +s q%0.0 1 nm -1 (2%0.0578 deg).

Small angle resolution

'S4/S

'S4/S


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0.02 0.0 2 0.0 2 0.082

10 110 2

10 3

10

10 5

10(cps)

q(1/nm)

200nm 750nm

USAXS Profile

10 0

Colloidal silica USAXS

e s +pe o t e s , c+ +s+ssumed to e sp er c+,.

e + er+ge p+rt c,e s 4eme+sured y U !" +greed

t +,ues o t+ ned us ng t e, g t sc+tter ng met od n ots+mp,es.

e concentr+t on o s , c++s 5 t n ot s+mp,es. e

sc+tter ng ntens ty ec+mestronger +s p+rt c,e s 4e

ncre+sed.

sample 'S4/S ight scattering

a#erage a#erage

@$$nm 19) 19

5$nm @

'S4/S

I 0 l


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Ahat;s in0plane /R3 L! "bser#ation of planes perpendicular to the surface

! *easurements of ultra0thin films! 4pplication to pole figure measurement

*i--raction angle BraggIncidence #7ray Re-lected #7ray

*i--racted #7ray

ut o" Plane

In Plane

In0+lane/R3

I 0 l


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$

1$

@$

)$

I$

5$

5 1$ 15 @$ @5 )$ )5 I$ I5 5$ 55 F$@ > deg. ?

I n t e n s

i t y

> & + S

?

x 103

+entacene 5$nm

In0plane

)0dimensional structure analysis

+C


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+robed depth control

Sample 4l Aa#elength 1.5 $5 ) &uM 1

10

100

1000

e * t i n $ t

i o n

d i s t a n $ e

! n m

(

1 00 +0 ,0 40 20 0

in$ident an'le !de'#ee(

0 0001

0 001

0 01

0 1

1

In0+lane/R3

I 0+l


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- ample 1

2-0

200

1-0

100

-0

0

. n t e n s

i t y

! $ & s (

+0/0,0-04030

2 / !de'#ee(

lan$in' An'le 0 2 de'#ee

0 - de'#ee

Al u

Al u

u!111( u!200(

u!220(

Al!111(

Al!220(

Al!311( Al!222(

4l interface layer 4lK&u

&u

7aSi" @

)$$nm

Si >substrate?

&E304l layer for %iring 4l0&u alloy transition layer %as detected.

K K In0+lane

In0+lane/R3

I 0+l


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Ag / FePt (01 nm) / 2lass

< 7 8 nm t ick &g top layer=

:lass sub.Fe+t

4g cap

1- nm

1 nm

E1ample 9

-#aluation of Fe+t magnetic thin film

K K In0+lane

In0+lane/R3

I 0+l


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Out-of-Plane diffraction profiles for samples with Ag top layer

0

-00

1000

1-00

2000

2-00

3000

3-00

4000

4-00

-000

20 30 40 -0 ,0 /0 +0

2th out de'

. n t e n s

i t y

3 a u 4

A' 0 nm

A' 0 2- nm

A' 0 -nmA' 1 0nm

5a#o f#om 'lasssubst#ate is ob6ious

Only 7e8t!111( $an be obse#6ed f#omthin film laye#

9he#e is no s&e$ifi$obse#6ation f#om A'$a& laye#

E1ample 9-#aluation of Fe+t magnetic thin film

In0+lane/R3

In0+lane


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!A&&l 8hys ett +3 21;, !2003((@$ )$ $ 5$ $ $ $

3iffraction angle @ / Ndeg.O

I n t e

n s

i t y

N a r

b .

u n

i t O Fe+t >fcc

fct?

Fe+t >fct?

4g>111?

%ith 4g cap

no 4g cap

-#aluation of Fe+t magnetic thin film

Fe+t e pected as a high density magnetic recordingmedia

:lass sub.

Fe+t >fct? 15nm 4g cap 1nm

:lass sub.Fe+t >fcc? 15nm

E1ample D

!A&&l 8hys ett +3 21;, !20

K K In0+lane

In0+lane/R3

fct >face centered

tetragonal?

fcc >face centered

cubic?

In0+lane


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*otion of goniometer in polefigure measurement by standard

sample hori6ontal goniometer

Incident /0ray

Diffraction X-ray

Pa is

Sample

Flapping motion of sample is easy to understandbecause this is managed by one a is >chi a is?.

7here is loss of intensity in position ofQ $degree In+lane measurement ,asincident line focus /0ray and sample surface

makes perpendicular layout.

rotation axis

*otion a es are Pa is>step? a is>scan?

Sample is inclined sosample is not kept

hori6ontally.

In0+lane/R3

In0+lane


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+ole figure measurement in sample hori6ontal Tin0planeUgoniometer

Incident X-ray

Diffracted X-ray

10mm

Incident X-rayeam !idt" #

1$0mm %&

Detect'r

(ara))e) *)it+na)y,er

.

(at" 'fdetect'r

(at" 'f Incident'/tic

4t all time a ample is kept hori6ontally It i /' i2)e t' mea 3re fr'm

In-/)ane t' '3t-'f-/)ane directi'n c'ntin3'3 )y

4 r'tati'n5axi

6ecei7in8 )it%$0mm 9 %0mm 'r

(ara))e) *)it +na)y,er

In0+lane/R3


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-#aluation of thin films

"rganic film

3ielectric film&ompound

semiconductor

*agnetic film

Single crystal%afer

&rystal structure

7e ture

&rystallinity

7hickness

+article < poresi6e

"ptics LL

*ethodLL


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-#aluation of thin films

"rganic film

3ielectric film

&ompoundsemiconductor

*agnetic filmSingle crystal

%afer

&rystal structure

7e ture

&rystallinity

7hickness+article < pore

si6e


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Selecting application

Select application


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Sample alignment

Smart ab

5 simple parameters


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Sample alignment

Smart ab

5 simple parameters

*anual setting)5 arameters


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*a imum fle ibility


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"ptical component sensors

*arks

+hoto sensors

:e>@@$? @ K Soller slit


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Smart ab

Setting up optics

Arong parts are sensed and indicatedVV


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*easurement

Casic file and sample information


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4utomatic alignment

!Source height!Incident beamdirection!*irror angle!3i#ergence slit height

!Sample height!@ 6ero point!3etector setting


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TH&5+ .$ 0.R .$R &TTE5TI.5TH&5+ .$ 0.R .$R &TTE5TI.5

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Claudia_Gavrilescu_XRAY Technology.pdf