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You are on page 1of 35

Structure to Bulk Properties

Charles Glinka

NIST Center for Neutron Research

Gaithersburg, Maryland

(http://www.ncnr.nist.gov)

Techniques for the Measurement of Microstructure

Neutron

reflectivity

USANS

SANS or SAXS?

SANS SAXS

scattering scattering electron density

length density

SANS or SAXS?

SANS SAXS

Features H/D contrast for time-resolved

variation measurements

• Magnetic

•Superior Q-

scattering

resolution

• Conducive to

extreme •Anomalous

envivonments scattering

• nondestructive

•Small sample size

SANS or SAXS?

SANS SAXS

scattering to some samples

• H/D isotope

effects • Parasitic

scattering

• Fluorescence

• Beam stability

Concepts Common to SANS and Neutron Reflectometry

Scattered

Collimated beam of neutrons

monochromatic counted as a

neutrons incident on n

S

2θ function of

sample, S

vi pi ki scattering

scattering angle, 2θ

Sample

Incident neutron angle

r 2π

wave vector, ki =

λi Scattering Triangle ki - kf = Q

Q scattering vector

2θ

ki

For elastic scattering (ki = kf = 2π/λ)

r r r

Q = ki − kf

kf r

2θ Q Q = 2k sinθ

ki 4π

Q = sinθ

λ

2π λ 2π

or d= = =

2 sinθ 4π Q

sin θ

λ

In general, diffraction (SANS or NR) probes length scale

2π λ

d≈ , for small scattering angles, d ≈

Q 2θ

Center for Neutron Research

In general, diffraction (SANS or NR) probes length scale

2π λ

d≈ , for small scattering angles, d ≈

Q 2θ

r

structure in the direction of Q, on a scale, d ≈ 2π Q

ki r ki

2θ Q 2θ

kf kf

r cf. Appendix A.

same I(Q)

Center for Neutron Research

Diffraction Probes rStructure

r rin the Direction of Q

ki − k f = Q

Specular Reflection Geometry SANS Geometry

ki kf kf Q

ki 2

2 Q

Reflectivity probes

plane of sample (parallel to

structure perpendicular to

Q), and averages over

surface (parallel to Q), and

structure perpendicular to

averages over structure in

sample surface.

plane of sample.

SANS Instrument Schematic

2θ

a scale d , where

0.5 nm < λ < 2 nm (cold neutrons)

d ≈ λ (wavelength)

0.1° < θ < 10° (small angles)

2θ (scattering angle)

1 nm < d < 300 nm

SANS Fundamentals

• For Length Scale Probed by SANS Can Use Continuum Approximation

- consider H2O, v ~ 30 Å3, r ~ 2 Å

Scattering Length

Density

neutrons X rays

b Z re

• Therefore we can use material properties rather than atomic

properties when doing small-angle scattering

Center for Neutron Research

SANS Fundamentals

give rise to small-angle scattering

2

r 1 r rr r

I(q) = ∫ ρ (r )e iq⋅r

dr Rayleigh-Gans eqn.

V V

Entire volume of sample

SANS Fundamentals: Coherent vs. Incoherent Scattering

N 2

Consider scattering from N r 1 rr

A

atoms of a single element, Z X I(q) =

V

∑b e i

i

iq ⋅ri

X rays Neutrons

A1

A1 A1

A2

A1

A3 A2

A2

A2

electron

atomic radius atom scattering A3

number form factor lengths, b’s, A3

depend on isotope A3

and isotope spin

scattering length

Center for Neutron Research

SANS Fundamentals: Coherent vs. Incoherent Scattering

N 2

Consider scattering from N r 1 rr

A

atoms of a single element, Z X

I(q) =

V

∑b e i

i

iq⋅ri

N

r 1 (

r r r

)

∑ bi b j e

iq⋅ ri − r j

A1 I(q) = Since b’s are

V uncorrelated with

A2 i, j

the atom positions

neutron r 1 N iq⋅(ri − r j )

r r r r r

A3

I(q) = ∑ bi b j e = ICoh (q ) + I Incoh (q )

V i, j

where structural

N

r 1 (

r r r

)

∑

A1 A2 2 iq⋅ ri − r j information

A1 A2 ICoh (q) = b e

A1 A2 V i, j

( )∑

N

A3 r 1 2 2 (

r r r

iq ⋅ r j − r j )

A3 I Incoh (q) = b − b e

A3 V j, j

scattering lengths: depend

on isotope and isotope spin

no structural 1

information

General Results for a Two-Phase System

refers to scattering

length density

From the Rayleigh-Gans equation:

2

r 1 rr r rr r

I(q) = ∫ ρ1 e iq⋅r

dr1 + ∫ ρ 2 e iq⋅r

dr2 break total volume

V V1 V2 into two sub-volumes

2

r 1 iq⋅r r

rr iqr ⋅rr r iq⋅r r

rr

I(q)= ρ1 ∫ e dr1 + ρ 2 ∫ e dr − ∫ e dr1

V V1 V V1

2

r 1 iq⋅r r

I(q) = ( ρ1 − ρ 2 ) ∫ e dr1

rr

2

V V1

Contrast Factor

(depends on materials Spatial arrangement

and radiation properties) of material

General Results for a Two Phase System

2

dΣ r 1 iq⋅r r

(q) = (ρ1 − ρ2 ) ∫ e dr1

rr

2

dΩ V V1

‘Particles’(i.e. discrete

Non-particulate systems

inhomogeneities)

r − iqr⋅rr r

I(q ) = ( ρ1 − ρ 2 ) F(q) S(q) I(q) ∝ ( ρ1 − ρ2 )

N

∫ γ ( r )e

2

2 2

dr

V V

single particle

contrast

shape correlation function

2 interparticle

r

rr

∫

iq ⋅ r correlations

e dr

Vp

Scattering Invariant

10 % black

90 % white

in each square

*Guinier and Fournet, pp. 75-81.

Porod Scattering

• At large q:

Porod Scattering

Center for Neutron Research

SANS and Thermodynamics

small-angle scattering

ρ2

I(0) = kT β T Isothermal compressibility

V

Composition fluctuations also produce small-

angle scattering

I(0) = kT /

V ∂φ 2

Multi-Phase Materials

as for 2 - phase systems

Center for Neutron Research

Multi-Phase Materials

possibly many unknown Sij’s

*Higgins and Benoit, pp. 121-122.

Center for Neutron Research

Solving Multi-Phase Structures

Contrast Matching

reduce the number of phases “visible”

ρ solvent = ρ core

(shell visible)

or

(core visible)

ρ solvent = ρ shell

Contrast Variation

of known contrasts and unknown ‘partial structure functions’

• Sturhmann Analysis

Determine structure from Rg = f (contrast)

NIST Center for Neutron Research (NCNR)

• 20 MW Reactor (4 x 1014 n/cm2-s • 21 beam facilities (7 thermal, 14 cold)

peak thermal flux)

• 6 irradiation facilities

• Large liquid H2 cold source (25 K)

SANS Instrumentation at the NCNR

CHRNS 30-m SANS

8-m Pinhole SANS 0.010 nm-1 < Q < 6 nm-1

0.05 nm-1 < Q < 0.5 nm-1

Perfect-Xtal USANS 30 m

5 x 10-4 nm-1 < Q < ~ .01 nm-1 NIST / ExxonMobil 30-m SANS

0.008 nm-1 < Q < 7 nm-1

SANS Instruments at the NCNR

1992

Triple-bounce

Detector

analyzer xtal

shielding

USANS Instrument

SANS APPLICATIONS

POLYMERS:

• Conformation of Polymer Molecules in Solution and in the bulk

• Structure of Microphase-Separated Block Copolymers

• Factors Affecting Miscibility of Polymer Blends

BIOLOGY:

• Organization of Biomolecular Complexes in Solution

• Conformation Changes Affecting Function of Proteins, Enzymes, DNA/Protein

complexes, Membranes, etc.

• Mechanisms and Pathways for Protein Folding and DNA Supercoiling

CHEMISTRY:

• Structure and Interactions in Colloidal Suspensions, Microemulsions,

Surfactant Micelles, etc.

• Microporosity of Chemical Absorbents

• Mechanisms of Molecular Self-Assembly in Solutions and on Surfaces

of Microporous Media

Using Deuterium Labeling to Reveal Polymer Chain Conformation

bD

I(Q) ∝ c (b H − b D ) P (Q) 2

bH

" Form Factor"

N z rr

∑∑ e

1 iq ⋅ri , j

P (Q) = 2

z i j

- if labeled chains are randomly dispersed

I(Q) ∝ x (1 - x) (b H − b D ) 2 P(Q)

homopolymer blend

I(Q) ∝ ( x b D + (1 - x)b H ) 2 ST (Q) +

x (1 - x) (b H − b D ) 2 P (Q)

Can determine ST and P(Q) from 2 measurements, with different fractions (x) of labeled chains

SANS APPLICATIONS

METALS AND CERAMICS:

Fatigue or Radiation Damage

MAGNETISM:

• Magnetic Ordering and Phase Transitions in Ferromagnets, Spin Glasses,

Magnetic Superconductors, etc.

General References: SANS and SAXS

By R.-J. Roe, Oxford University Press (2000).

Amorphous Bodies, A. Guinier, Dover Books (1994).

Fournet, John Wiley & Sons (1955).

Benoit, Clarendon Press-Oxford (1994).

Small Angle X-Ray Scattering, O. Glatter and O.

Kratky, Academic Press (1982).

Center for Neutron Research

Appendix A. Scattering from Two Nuclei

∆d

d Ψscat

∆φ = 2π

λ

r r r r

kf ∆φ = r ⋅ ki − r ⋅ k f

1

r r r

incident

neutrons

r Q ∆φ = r ⋅ (ki − ⋅k f )

r r

∆φ = r ⋅ Q

2

ki

b1 ikR b 2 i ( kR + ∆φ )

Ψscat =− e − e Scattered wave function

R R

SAS of X rays - Guinier (1955), Ch.1

for N nuclei

Polymers and Neutron Scattering,

Higgins & Benoît (1994), p.11

N 2

r r

dσ 1

=

dΩ N ∑b e

1

i

iQ⋅ ri

Appendix A. Scattering from N Nuclei

N r r

dσ 1 neutrons scattering in

=

dΩ N ∑b e 1

i

iQ⋅ ri

direction corresponding to

Q, divided by # incident per

unit area

r r r Only components

ri = r// + r⊥ r

ri of ri parallel to Q

r r r contribute to

Q ⋅ ri = Q r// Q summation

direction of Q only!!

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