modelling data – better approaches how to get … - neutron...some scattering at interfaces x-ray...
TRANSCRIPT
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Modelling Data –
Better Approaches How to get useful information?
Adrian R. Rennie
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Monolayers –
Simple Interpretation
0.0E+00
1.0E-07
2.0E-07
0.00 0.01 0.02 0.03 0.04 0.05
Q2 / Å-1
gs(Q
) / Å
-2
8 Å15 Å20 Å30 Å60 Å
Define gs
(Qz
) in terms of measured reflectivity and RF
(Qz
) (the Fresnel reflectivity for perfectly sharp
interface):
gs
(Q) = Q2
(R
−
RF
) / (1 − R)
ln
gs
(Q) ≈ –t2
Q2
/12
Roughly ln
(Q2
R)
≈
–t2Q2/12
Contrast match of two bulk phases RF
(Q) = 0
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Real Interfaces are not just layers
Slab models are easy to calculate but people are not very interested in just thickness and scattering length density
1 2 3 4
Top
Sub
Neutron beam
Solid
Roughness Top 1 2 3 4 5 6 7 8
Liquid F reg 1
F reg 2
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Surface Excess and Area per Molecule
Volume per molecule: Vm
Scattering length:
bmScattering length density:
= bm
/ Vm
Thickness of layer:
tScattering length density
Area per molecule:
AmVm
= t AmScattering length density:
= (bm
/ Vm
) = bm
/( t Am
)
Area per molecule:
Am
= bm
l
t
a l
t
T S
Neutrons
Am
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Adsorption of SurfactantSurface active moleculesAmphiphilicBind to surface –
how?
What are properties?
Hexadecyl trimethyl ammonium bromideC16
H33
N(CH3
)3+
Br-
Tail Head
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Some Possible Structures
•
Monolayer
•
Bilayer
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Cationic Surfactant
CTAB at 27°
C on amorphous SiO2
(a) D2
O (b) cmSiO2
at 6 ×10-4
M ModelsSolid line –
Bilayer
Dashed line -
Monolayer
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Cationic Surfactant
•
CTAB
27 C on SiO2
•
Label heads & tails
Head 6 +/-
2 ÅTail 28 +/-
4 Å
Roughness ~ 8 ÅFractional Coverage35% at 3 ×10-4
M
80% at 6 ×10-4
M Langmuir
6, 1031-1034 (1990).
J. Colloid Interf. Sci.
162, 304-310 (1994).
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Plotting Data
1.0E-06
1.0E-05
1.0E-04
1.0E-03
1.0E-02
0.0 0.1 0.2 0.3
Q / Å-1
Ref
lect
ivity
Lipid DSPC
Background
1.0E-06
1.0E-05
1.0E-04
1.0E-03
1.0E-02
0.0 0.1 0.2 0.3
Q / Å-1
Ref
lect
ivity
Lipid DSPC - Bgd subtracted
-1.0E-08
1.0E-08
3.0E-08
5.0E-08
0.0 0.1 0.2 0.3
Q / Å-1
RQ
4
Lipid DSPC - Bgd subtracted
Different representation is helpful
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How to Look at Data?
Log10
R vs Q RQ4
vs Q
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Effects of Resolution
-4
-3
-2
-1
0
0.00 0.05 0.10
Q / Å-1
log 10
R1%
3%
5%
7%
Silicon substrate: film thickness 1500
Åscattering length density 6.3
×
10−6
Å-2
Q/Q
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Non-Uniform SurfacesIf you have patches of different layers at an interface do you average the density or average the reflectivity?
1 2 3 4
Top
Sub
Neutron beam
Solid
Roughness Top 1 2 3 4 5 6 7 8
Liquid F reg 1
F reg 2
What is the coherence length of a neutron?
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Describing Polymers
•
Interdiffusion –
is this roughness?•
Brushes –
parabolic density profile
(E. P. K. Currie et al Physica
B,
283
17 –
21)•
Other scaling laws e.g. O. Guiselin J. Phys.
50, 3407-3425 (1989).
We expect smooth profiles!
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Thermoresponsive polymer brush
J. Zhang, et al., Soft Matter, 4, 500–509 (2008).
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Repeating Layers
A one dimensional crystal
Bragg’s law
Intensity of peaks mayDepend on size and disorder
Sub Liquid
1 2 3 4
Top
Neutron beam
Solid
Roughness Top 1 2 3 4
Bilayer N repeats
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Calculate reflectivity for a profile
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Using Multiple Contrasts
Simultaneous fits for multiple data sets
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Off-specular Scattering, GISANS, Near- surface SANS
Adrian R. Rennie
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Interfaces are 3-dimensional
Understanding rheology –
shear flow
Brown et al.
Progress in Colloid and Polymer Science 98, (1995) 99-102.
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Fate of a Neutron at an Interface
•
Reflected•
Scattered/Diffracted from surface
•
Absorbed•
Scattered from bulk (either side of surface)
•
Other accidents
NeutronsNeutronsNeutronsNeutronsNeutronsNeutrons
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Evanescent Wave
Below kc
no travelling wave enters the sample
Amplitude decays with depth in sample
Decay length depends on (c
-
)
Evanescent wave can cause scattering
-2000
-1500
-1000
-500
0
-1 -0.5 0 0.5 1
z / Å
neutrons c
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Looking at Materials
Anneli
Salo
-
Own work, CC BY-SA 3.0, https://commons.wikimedia.org/w/index.php?curid=6746303
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Looking at Materials
Anneli
Salo
-
Own work, CC BY-SA 3.0, https://commons.wikimedia.org/w/index.php?curid=6746303
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Off-specular & Reflection
Frédéric
Ott, Sergey Kozhevnikov
‘Off-specular data representations in neutron reflectivity’, J. Appl. Cryst. 44, (2011), 359-369.
Qz
≈
(2π/λ) (θi
+ θf
)
Qx
≈
(2π/λ) (θi
+ θf
) (θi
- θf
)(2012),
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Scattering from Surface Structures
Peter Müller-Buschbaum
‘GISAXS and GISANS as metrology technique for understanding the 3D morphology of block copolymer thin films’
European Polymer
Journal
81, (2016), 470-493.
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10% vol. dispersion, Radius ~350 Å. Sapphire substrate, i
= 0.35 deg
1.5
1.0
0.5
0.0
1.5
1.0
0.5
0.01 2 3 4 5 6
-0.2
0
0.2
0.4
0.6
0.8
1
1.2
1.4
1.6
(Ang.)
(d
eg)
96083
-4.5
-4
-3.5
-3
-2.5
-2
0 2 4 6
/ Å
f/ d
egre
es
PS latex in D2
O Liquid/Sapphire
Strong Off-specular Scattering
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PS latex in D2
O Liquid/Sapphire
10% vol. dispersion, Radius ~350 Å, sapphire substrate, i
= 0.35 deg
Transform to map of Qz
Qx5
10
0
-5
0.01 0.02 0.03 0.04Qz
/ Å-1
Qx
/ 10-5
Å-1
5
10
0
-5
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Some Scattering at Interfaces
X-ray scattering – glass
Sinha et al., Phys. Rev. B.
38, 2297, 1988.
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Scattering from D2
O
and from null reflecting water
(8% D2
O)0
10
20
30
40
50
60
70
80
-1 0 1 2 3 4
Angle, / degrees
Ave
rage
Cou
nts
Rennie et al., Macromolecules
22, (1989), 3466-3475.
Incoherent background
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Interfacial structure: GISANS
Nouhi
et al. Journal of Applied Crystallography (2017)
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Calculating ScatteringDistorted Wave Born Approximation (DWBA)
Simply allow for sequential events e.g.
Reflection then ScatteringRefraction then ScatteringScattering then Reflection
Reflect only
Reflect and Scatter
Reflection followed by weak scattering.
(a)
Optical Matrix Calculation
(b)
Weak Scattering (Born approximation)
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How deep is the evanescent wave?
0
500
1000
1500
2000
0.0 0.2 0.4 0.6 0.8 1.0Incident Angle / degrees
Evan
esce
nt W
ave
Dep
th /
Å
16 Å
14 Å
12 Å
10 Å
8 Å
6 Å
0
500
1000
1500
2000
0 5 10 15 20
Wavelength / ÅEv
anes
cent
Wav
e D
epth
/ Å
0.37 degs
0.62 degs
Silicon/D2
O Interface
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Copolymer films
P. Müller
Buschbaum
et al. J. Appl. Cryst. 47, (2014), 1228–1237
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Changes with DepthHorizontal cuts
•
Used wavelength to probe different depths
•
Longer wavelength looks neare
the
surface
J. Appl. Cryst. 47, (2014), 1228–1237
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Diffraction from Surface Layers
Nouhi
et al. Journal of Applied Crystallography
(2017)
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Penetration depth
A depth sensitive technique:
Wavelength Incident angle
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Data at different angles
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Data at different angles
z1/e
<z1/e
>
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Calculations & Intensity Data
QCM-D data: structure forms with a separation from the interface [Hellsing
et al. 2017, manuscript]
D22 -
ILL
NG3 SANS -
NCNR
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Scattering at Interfaces
•
Off-specular scattering•
Near Surface SANS
•
GISANS
What is the difference?
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PS latex in D2
O Liquid/Sapphire
10% vol. dispersion, Radius ~350 Å, sapphire substrate, i
= 0.35 deg
Transform to map of Qz
Qx5
10
0
-5
0.01 0.02 0.03 0.04Qz
/ Å-1
Qx
/ 10-5
Å-1
5
10
0
-5
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PS latex in D2
O – sapphire surface
10% vol dispersion, 0.35
Sum along Qx
0.001
0.01
0.1
1
0 0.01 0.02 0.03 0.04 0.05 0.06 0.07
Q / Å-1
R(Q
)
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PS latex in D2
O – sapphire surface
10% vol dispersion, 0.35, 0.8 and1.5 deg
Assign Bragg peaks (index)
Q1
= 0.00282 Å-1
d = 2230 Å
3 first peaks outside range
y = 0.002820x - 0.000360
0.00
0.01
0.02
0.03
0.04
0 2 4 6 8 10 12 14
Order of Peak
Qpe
ak /
Å-1
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PS latex in D2
O – sapphire surface
10% vol dispersion, 0.35
Sum along Qx
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0 0.01 0.02 0.03 0.04 0.05 0.06 0.07
Q / Å-1
R(Q
)
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Compare Qx and Qz
M. S. Hellsing, et al. Applied Physics Letters, 100, (2012), 221601.