Small Angle X-ray Scattering

(SAXS)
Outline
1. SAXS overview
2. SAXS Experiment
1. X-Ray source
2. Beam path instrument
3. Detector
3. SAXS Theory
1. Basic principle
2. Importance of small angle
3. Interpretation
SAXS Overview
elastic scattering
x-ray wavelength
0.01 - 0.2 nm
detection angle
0 - 10
distance probe
nanometers to
micrometers
O..Glatter, O. Kratky. Small Angle X-Ray Scattering
Academic Press, 1982.
SAXS Overview
John A. Pople. Everything You Ever want To Know About SAXS But Were Afraid To ASK
(http://www-ssrl.slac.stanford.edu/conferences/workshops/scatter2006/talks/pople_saxs_workshop_060522.pdf)
SAXS Experiment : X-ray source
X-ray is high energy electromagnetic wave
(25 keV per photon @ 0.05 nm wavelength)
Conventional X-ray source : X-ray tube
X-ray tube @ wikipedia
(http://en.wikipedia.org/wiki/X-ray_tube)
SAXS Experiment : X-ray source
X-ray is high energy electromagnetic wave
(25 keV per photon @ 0.05 nm wavelength)
Conventional X-ray source : X-ray tube
X-ray tube @ wikipedia
(http://en.wikipedia.org/wiki/X-ray_tube)
SAXS Experiment : X-ray source : Synchrotron
Synchrotron light source
high intensity
high collimation
(small divergence)
wide wavelength
tunability
SPring-8, Hyogo prefecture, Japan
SAXS Experiment : X-ray source : Synchrotron
Synchrotron light source
high intensity
high collimation
(small divergence)
wide wavelength
tunability
How do synchrotron work?
www.diamond.ac.uk
SAXS Experiment : X-ray source : Synchrotron
D. Atterwood, Synchrotron Radiation Berkley University lecture presentation
SAXS Experiment : X-ray source : Synchrotron
Insertion devices
Undulator @ wikipedia
(http://en.wikipedia.org/wiki/Undulator)
c m
eB
K
e
u
T
P
2
=
undulator
1
wiggler
1 >>
SAXS Experiment : X-ray source : Synchrotron
Insertion devices
c m
eB
K
e
u
T
P
2
=
undulator
1
wiggler
1 >>
D. Atterwood, Synchrotron Radiation Berkley University lecture presentation
SAXS Experiment : X-ray source : Synchrotron
Emitted photon energy
bending magnet & wiggler
undulator
m B e E
c
2 / 3
2
, J =
) ( ) ( 6650 . 0 ) (
2
T B GeV E keV E
c c
=
) )
2 2 2 2
) 2 / ( 1 2 / j , , P P = K
u
)
2 2 2
2
) 2 / ( 1 ) (
) ( 9496 . 0
) (
U , + + K c
e
ke
u
e
SAXS Experiment : Beam path instrument
Optical system (monochromator, collimator)
D. Atterwood, Synchrotron Radiation Berkley University lecture presentation
SAXS Experiment : X-ray detector
sequential mode vs parallel mode
sequential
parallel
O..Glatter, O. Kratky. Small Angle X-Ray Scattering Academic Press, 1982.
SAXS Experiment : X-ray detector
gas-filled radiation detector
scintillators
semiconductor detectors
photographic plate
novel detectors (CCD, solid state)
SAXS Theory : Basic Principle
Radiation Visible light X-rays Neutrons
Type
Electromagnetic
wave
Electromagnetic
wave
Particle/Wave
Wavelength 400-700 nm 0.01-0.2 nm* 0.01-2.0 nm*
Distance probed >0.01 m nm to m nm to m
Scattered by
variations of
refractive index electron density
nuclear scattering
properties
* the wavelengths which used in scattering technique, not the entire region of radiation
SAXS Theory : Basic Principle
Scattering cross section of X-rays and neutrons
J. M. Carpenter Introduction to Theory of Neutron Scattering Presentation at Argonne National Laboratory, 2006
SAXS Theory : Basic Principle
light scattering
2
scattering vector (Q)
Incident beam transmitted beam (k)
scattered beam (k)
detector
k k Q
T T T
= '
P
j T sin 4
= Q
SAXS Theory : Importance of small angle
from Braggs law, distance probed is inversely proportional to Q
Q
d
T
U
2
sin 2
! !

U T sin 4
! Q
;
high Q : intra-particle, atomic level data
low Q : inter-particle, colloidal level data
since wavelength > 0.2 nm tend to
absorbed strongly, small angle is
needed for colloidal system
SAXS Theory : Importance of small angle
WAXS vs SAXS
theoretically same experiment
with different condition
experimentally have some
difference in instrument design
WAXS
SAXS
John A. Pople. Everything You Ever want To Know About SAXS But Were Afraid To ASK
SAXS Theory : Interpretation
Extracting data from scattering
Q
I(Q)
Q
I()

SAXS Theory : Interpretation : Size of Particles

Scattering pattern for dispersed colloid system
)
)
)
2
3
cos sin 3
)
`

|

!
QR
QR QR QR
Q P
) ) ) Q P V N Q I
P P M P
2
2
V V =

P

M
for spherical particle,
SAXS Theory : Interpretation : Size of Particles
Scattering pattern for dispersed colloid system
)
)
)
2
3
cos sin 3
)
`

|

!
QR
QR QR QR
Q P
) ) ) Q P V N Q I
P P M P
2
2
V V =
for spherical particle,
T. Cosgrove Colloid science : Principle, methods
and applications Blackwell Publishing, 2005
SAXS Theory : Interpretation : Polydispersity
polydispersity gives multiple R value, promote smearing
)
)
)
2
3
cos sin 3
)
`

|

!
QR
QR QR QR
Q P
T. Cosgrove Colloid science : Principle, methods and applications Blackwell Publishing, 2005
SAXS Theory : Interpretation : Shapes
Guiniers law : approximation for Q < 1/R
G
a R
G

5
3
3 / exp
2 2 2 2
G P P
R Q V N Q I ( ! V

!
V
G
dV r
V
R
2
//
;
2
r
R
G
!
12
I
R
G
!
T. Cosgrove Colloid science : Principle, methods and applications Blackwell Publishing, 2005
SAXS Theory : Interpretation : Surface area
Porod law : approximation at high Q
)
4 2
2

A ! SQ Q I V T
) ) ) Q D A Q I
s
ln 6 ln =
;
2
R area w 2 =
s
D
3
area w 3 !
s
T. Cosgrove Colloid science : Principle, methods and applications
Blackwell Publishing, 2005
References
1. O.Glatter; O. Kratky Small Angle X-Ray Scattering Academic Press,
1982.
2. L. Feigin; G. Taylor Structure Analysis by Small Angle X-ray and Neutron
Scattering Plenum Press, 1987.
3. D. Attwood Synchrotron Radiation for Materials Science Applications
lecture presentation (available at http://ast.coe.berkeley.edu/srms/)
4. J. Pople Everthing You Ever Wanted to Know About SAXS But Were
Afraid to Ask SSRL workshop
(available at http://www.camd.lsu.edu/Workshops/JohnPople.pdf)
5. T. Cosgrove Colloid science : Principle, methods and applications
Blackwell Publishing, 2005