A Study on Parasitic Slit-Scatterings

in SAXS Equipment
Tuo Huang
Grinnell College, IA, USA
PI!entor" #r$ %ouli &i
!aterials 'esearc( &a)oratory, Uni*ersity o+ Cali+ornia, Santa ,ar)ara, CA, USA
August -../, Uni*ersity o+ Cali+ornia, Santa ,ar)ara
I$ Introduction
T(e X-'ay #i++raction 0X'#1 2acility is one o+ t(e most +requently used user-
+acilities la) at !'&, UCS,$ ,y using X-ray di++ractometers, researc(ers 3(o 3or4
3it( nanosystems, suc( as organicinorganic(y)rid crystals, )iomacromolecules,
semiconductor de*ices, polymers, micro+i)ers, etc, are a)le to o)tain in+ormation
a)out t(e nanoscale structures o+ t(eir materials$ Among t(e many X'# tec(niques,
Small Angle X-ray Scattering 0SAXS1 is )est suited +or e5amining nanostructures on
t(e scale o+ 6.
6
to 6.
-
7$ In SAXS instruments, incident X-ray )eam must )e 3ell
collimated and (a*e a clear edge, so t(at user can clearly distinguis( t(e scattering
signals +rom t(e transmitted direct )eam$ To o)tain suc( a )eam pro+ile, multiple
apertures +ormed )y pairs o+ (ori8ontal and *ertical slits made o+ (ea*y metals suc( as
tantalum or tungsten, 3(ic( are strong 5-ray attenuators, are used to de+ine t(e
geometrical s(ape and si8e o+ t(e )eam$
6
Ho3e*er, slits made +rom suc(
polycrystalline metals, no matter (o3 +inely mac(ined and polis(ed, 3ill generate
undesira)le 9parasitic scattering9, 3(ere slits t(emsel*es scatter X-ray p(otons in a
3ide angle and produce strong )ac4ground noise in t(e )eam pro+ile$
In t(is researc(, 3e conducted a series o+ e5periments to c(aracteri8e t(e slit
scattering +rom di++erent materials under *arious conditions in order to +ind possi)le
3ays to en(ance t(e per+ormance o+ SAXS instruments$
Page 2 12
II. Experiment Approaches
:e +irst studied t(e scattering pro+ile o+ traditional tungsten )lades +rom actual
5-ray slits 3idely used in 5-ray di++ractometers 02igure 61$ ;ne o+ suc( slits 3as
placed at t(e sample-(older o+ t(e SAXS instrument and mo*ed across t(e 5-ray )eam
to produce slit-scattering images 0t(e incident )eam is normal to t(e edge o+ t(e slit1$
,e+ore t(e image 3as ta4en, an X-ray pin-diode 3as placed rig(t )e(ind t(e slit to
measure t(e X-ray )eam intensity 3(en t(e slit 3as mo*ed to a certain position$

Page 3 12
Scattered
Beam
(To detector)
Incident
Beam
Slit moves into the beam
2igure - s(o3s t(at as t(e slit cuts across t(e )eam 0t(e slit mo*es in negati*e 5
direction1, t(e X-ray intensity drops )ecause a larger part o+ t(e )eam is )loc4ed$ T(e
plot a)o*e also s(o3s t(at, on t(e inter*al 3(ere t(e intensity is )et3een <... and
-.... 0counts per second1, intensity drops linearly, 3(ic( means t(at t(e slit is
cutting into t(e central part o+ t(e )eam$ T(is inter*al is c(osen +or data-ta4ing so t(at
scattering at di++erent cutting-dept( (appen on t(e same lengt(-inter*al on t(e edge o+
t(e slit$
A+ter ta4ing t(e intensity-dept( plot, t(e pin-diode is remo*ed, and t(e slit is
dri*en to selected points o+ cutting-dept(s )y (ig(-precision stepping-motors
0accuracy 3it(in 6. microns1 and a t3o-dimensional scattering image 3as ta4en at
eac( point 3it( a multi3ire 5-ray area detector 0,ru4er HISTA'1$
T(e a+orementioned steps 3ere t(en repeated, only replacing t(e tungsten slit
3it( a piece o+ silicon 3a+er, 3it( its 6 . . crystal plane +acing t(e )eam and . . 6
plane on t(e edge 0so slit scattering, i+ any, s(ould occur on t(e . . 6 plane1$
Fig. 3: Experiment with Silicon wafer

T(e scattering pro+ile o+ silicon 3a+er s(o3s reduced slit-scattering, )ut t(e
scattering +rom t(e 3a+er=s edge still +its into a &orent8ian +unction$ Attempts 3ere
made to polis( t(e 0. . 61 plane +or greater +latness )ut t(at did not yield muc(
impro*ement$ Ho3e*er, 3e noticed t(at t(e 06 . .1 plane 3as *ery 3ell polis(ed
Page 4 12
(1 0 0) Plane
(0 0 1) Plane
Incident X-ray Beam
3(en t(e 3a+er 3as produced> t(ere+ore, i+ 3e could ma4e 06 . .1 plane instead o+ 0.
. 61 plane on t(e edge, scattering may )e signi+icantly reduced$
T(is resulted in ma4ing a tungsten slit 3it( a tiny strip o+ silicon 3a+er mounted
on t(e edge 02igure ?1$ T(is (y)rid slit 3as again tested using t(e same met(od as
a)o*e$
III. Results and Analysis
1. Tungsten Slit & Single!rystal Silicon Slit
To e5plain t(e analysis o+ scattering pro+ile, let us ta4e t(e image o+ tungsten slit
at position 5@-A$6/ and intensity I@6-B-/ Countssec as an e5ample$ All t(e ot(er
images ta4en are processed in t(e same manner$
T(e image is +irst displayed +rom t(e ra3 data +ile 02igure <1$ A+ter +inding t(e
pi5el position o+ t(e )eam center 0<C/$-<DA, <DB$A.-C1, a rectangular area is de+ined
along t(e X direction i$e$ t(e direction o+ t(e scattering Etail$F
Fig. 5: Analyzing the Scattering Tail
Page " 12
Tungsten Slit
Silicon Waer
1-0-0 Plane
Incident X-ray Beam
Fig. 4: Hybri Slit
T(en numerical integral is computed along t(e X a5is o+ t(e image to re+lect t(e
a*erage intensity o+ t(e points in t(e rectangular at eac( 5 position$ T(e resulting plot
is s(o3n in 2igure A$ In t(e plot, 5 a5is is t(e --t(eta scattering angle t(at eac( point
corresponds to 0la)el on 5 a5is is in re*erse order, and t(e pea4 corresponds to t(e
scattering EtailF in t(e image1"
Page # 12
Fig!re ": #e$!lt of %!merical &ntegration along the x'axi$
T(e result is t(en e5ported to a t3o-column c(iplot +ile t(at can )e read )y
analysis so+t3are suc( as !S E5celG or ;riginG$ T(e data 3as +urt(er assorted and
t(e data points t(at are on t(e scattering EtailF 3ere e5tracted to )e studied alone +or
cur*e +itting$
T(e scattering pro+iles o+ )ot( tungsten and Silicon :a+er slits +it into a
&orent8ian +unction in t(e +orm o+ 3(ere A and H are
*aria)les positi*ely correlated to t(e (eig(t and 3idt( o+ t(e pea4, respecti*ely$
2itting results are s(o3n in Ta)le 6 I -$
-
Page $ 12
Table (: )!r*e'+tting #e$!lt$ for the Scattering ,ro+le of
T!ng$ten Slit$
'elati*e
Slit
Position
0mm1
y. 5. H Error +or
H0J1
A Error +or
A 0J1
Goodness o+ 2it
'educed
K-square
'-square
.$6 .$D/<?? -.$6.<<< .$.BDC- .$...A- -$<<<BB .$.-C6- .$.-6- .$CC/A6
.$D .$6?.<? -.$6./66 .$.B6D< .$...<6 A$</B/< .$.A.66 .$6.C< .$CCB-B
.$< . -.$6.</A .$.//.C .$...?A 6?$?BC6C .$6DDC6 .$A.BD6 .$CCB.B
.$/ . -.$6.<< .$./-// .$...?A 6C$A-6DC .$6C-/B 6$-B/.C .$CC/C
.$C . -.$6.</ .$./.6- .$...?/ 6B$<6.DD .$6C-CD 6$DA6</ .$CC/A-
6$6 . -.$6.A6< .$.AB6< .$...<6 66$CD66C .$6D?.B .$/6-6? .$CC/6<
Table -: )!r*e'+tting #e$!lt$ for the Scattering ,ro+le of Silicon'
.afer Slit$
'elati*e
Slit
Position
0mm1
y. 5. H Error +or
H0J1
A Error +or
A 0J1
Goodness o+ 2it
'educed
K-square
'-square
.$6 .$??-?A -.$./</B .$.ACCB .$..-DC 6$<C<AA .$66C.- .$../6 .$CC-<C
.$D .$DAA6 -.$.AA?/ .$.A6/B .$..?6D D$-BD-? .$DDBCA .$.6./A .$CC<6/
.$< .$-?BDC -.$./D?- .$.A6/? .$..6/6 ?$<B-CA .$--A? .$.6-DB .$CCB.<
.$/ .$66DAA -.$./C.< .$.<<A/ .$..66D <$/6A.< .$--6?< .$.6C< .$CCB?C
.$C .$.6-?A -.$.B.B/ .$.?6BC .$..6/6 A$DA<</ .$?.C/ .$.D-/6 .$CC//-
6$6 . -.$.B//? .$.D?6< .$...B6 ?$A6D6? .$6/C6? .$.6?C6 .$CCB/6
2. %y&rid Slit
Lumerical integration 3as also done +or t(e images +rom t(e (y)rid slit and
compared 3it( t(e )ac4ground 02igure /1$ T(e negati*e (al+ on t(e (ori8ontal a5is
corresponds to t(e scattering tail on t(e image$ T(e pro+ile o+ t(e (y)rid slits 0)lue
cur*es1 are )asically superposed on t(e )ac4ground 0dar4-red cur*e1 i$e$ (a*ing
almost t(e same intensity 3it( t(e )ac4ground at eac( point, )ut only lo3er )ecause
Page ' 12
t(e o*erall intensity decreases as t(e slit mo*es +rom 5@ -A$- to 5@ -A$A, )loc4ing a
greater part o+ t(e )eam$ T(e pro+ile +rom t(e (y)rid slit is insigni+icant compared to
scattering +rom tungsten slits 0gold cur*e1$
D
Hence, 3e concluded t(at t(e (y)rid slit
(as no o)*ious slit-scattering$
I(. )iscussion
:e are not sure a)out 3(at (as caused t(e &orent8ian pattern in t(e scattering
tail, 3(ic( can also )e modeled )y a -- po3er +unction$ S$M$ Sin(a et al.
?
suggest t(at
it may )e due to t(e e5ponentially distri)uted roug(ness o+ t(e sur+ace and, in t(e case
o+ tungsten, also t(e randomly oriented polycrystalline micro-domains$
T(e a)sence o+ slit-scattering +or (y)rid slit is )ot( e5citing and 3ell 3it(in
e5pectation$ ,ecause t(e 06 . .1 plane is 3ell polis(ed and (as no roug(ness, 3(en
Page * 12
t(is plane is on t(e edge o+ t(e slit, t(e lo3est detecta)le 5-ray di++raction angle is t(e
one at AC$6D degrees +or t(e 0? . .1 plane 03(ic( is parallel to t(e 06 . .1 plane1$
<
%et
in SAXS, t(e X-ray )eam is collimated to a di*ergence angle o+ less t(an .$.< degrees
and t(e detection range o+ scattered angle is less t(an - degrees, )ot( o+ 3(ic(
c(aracteristics ma4e it impossi)le +or any X-ray p(otons scattered at a AC$6D-degree
angle to )e pic4ed up )y t(e detector$
(. !onclusion
A+ter studies on tungsten and silicon 3a+er slits, 3e can ma4e a tentati*e
conclusion t(at roug(ness o+ t(e sur+ace on t(e edge o+ t(e slit seems to )e t(e
primary cause o+ slit-scattering$ !ean3(ile, scatterings +rom polycrystalline micro-
domains also contri)uted to t(e o*erall slit-scattering and can )e reduced )y using
single-crystal material +or slits$ :(en )ot( +actors are ta4en care o+, as in t(e case o+ a
(y)rid slit, slit-scattering is reduced to undetecta)le le*el$
I+ +urt(er e5periments continue to s(o3 satis+actory results, t(ese ne3ly
designed (y)rid slits can lead to dramatic impro*ement to optical con+iguration o+ t(e
SAXS instrumentation$ In t(e traditional t(ree-slit setup, )esides t(e t3o set o+ slits
t(at collimate t(e X-ray )eam, additional slits are needed to cut o++ slit-scattering
+rom t(ose pre*ious slits$ In contrast, (y)rid slits do not generate slit-scattering and
t(us can signi+icantly simpli+y t(e design o+ SAXS equipment and )oost t(e
e++iciency and per+ormance o+ t(e equipment$
Page 1+ 12
(I. Ac,no-ledgements
It is a pleasure to ac4no3ledge t(e super) tec(nical assistance +rom Noanna
#ee4, Lic(olas Nudy and Eric :els(, and t(e (elp and guidance +rom t(e program=s
coordinator, #r$ Patricia Halpin and supermentor ,rett ,rot(erton$
T(is 3or4 3as supported )y t(e !'SEC Program o+ t(e Lational Science
2oundation under A3ard Lo$#!'.<--.?6<$
.otes and !itations
Page 11 12
1
N$ S$ Pedersen in Modern Aspects of Small-Angle Scattering edited )y H$ ,rum)erger 0Mlu3er Academic Pu)lis(ers,
#ordrec(t,oston&ondon, 6CC<1, </-C6
!
In cur*e-+itting, y. is +orced to )e 8ero i+ t(e automated +it returns a negati*e y. *alue, )ecause t(e )ac4ground o++set
cannot possi)ly )e negati*e in t(is case$
"
#ata +rom tungsten slit is not e5tracted +rom t(e ones analy8ed a)o*e, )ut 3as reta4en in t(e same set-up as t(e
(y)rid slit rig(t a+ter t(e (y)rid slit=s data 3as ta4en in order to s(o3 more *alid comparison$
#
S$ M$ Sin(a, E$ ,$ Sirota, and S$ Garo++$ P(ys$ 'e*$ , DB, --C/ - -D66 06CBB1
$
Latl$ ,ur$ Stand$ 0U$S$1 !onogr$ -<, 6D, D<, 06C/A1