Sample Detecto k k' Beam q = 4 π sin θ λ k' k q θ X-rays: Scatteri Neutrons: Scattering ~ μ nuclear , M perpendicu H Scattering Experiments
Sample
Detector
k
k'
Beam
q = 4 π sin θλ
k'
k
qθ
X-rays: Scattering ~ Z
Neutrons: Scattering ~ μnuclear, Mperpendicular
H
Scattering Experiments
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I(x) = I0 exp(−x /Lcoh )
Structural coherence length found for small regions from TEM images
SAXS: Structural Lcoh average
SANS: Structural and Magnetic Lcoh averages
Coherence Length
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λ =2dhkl sinθhkl
Observe diffraction from planes of particles at small angles
Both the lattice symmetry and the shape of diffracting object contribute to the intensity I(q
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I(q)∝ Slattice(q)Pshape (q,R)
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qhkl =4π sinθhkl
λBragg’s Law
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Psphere (q,R) =3(sin(qR) −qRcos(qR))[ ]
2
qR( )6
Ignore scattering by the surfactant coating
the radius R = Rcore
Small Angle X-ray Scattering
140
120
100
80
60
40
20
0
I (a.u.)
4.03.53.02.52.01.51.0
2θ
10
-8
10
-6
10
-4
10
-2
10
0
( )log P qr
0.50
0.50fcc
hcp
(100)
(002)
(101)
(110)
(103)
(112), (201)
(111)
(200)
(311), (222)
Both hcp and fcc arrays observed
Shape factor, d=8.5 nm
d=8.5 nm
x=10.3 nm
ShcpθP(θ)
ShcpθP(θ)
0
-2
-4
-6
-8
3D Arrays Structures from SAXS
d=8.5 nm
x=9.6 nm
2θ ( )Degree0.00.51.01.52.02.53.03.5 ( . .)Intensity a u05001000150020002500(002)(101)
( )a( )bSpots due to 3 hcp supercrystals- Large Lcoh
Interparticle spacing slightly reduced
(a) Average intensity
(b) Sharpest peak
3D Arrays Made Over 4 Weeks
Nanoparticle Crystals vs Disordered Assemblies
SAXS patterns of 8.5 nm Fe nanoparticle FCC nanoparticle crystals and rapidly quenched assemblies
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