Introduction to Inelastic Neutron Scattering Bruce D Gaulin … · 2017. 3. 13. · Magnetic...
Transcript of Introduction to Inelastic Neutron Scattering Bruce D Gaulin … · 2017. 3. 13. · Magnetic...
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Introduction to Inelastic Neutron Scattering
Bruce D Gaulin McMaster University
Neutrons: Properties and Cross Sections
Excitations in solids
Triple Axis and Chopper TOF Techniques
Practical concerns
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235U + n daughter nuclei + 2-3 n + gammas
neutrons:
no charges=1/2 massive: mc2~1 GeV
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6
Neutron interaction with matter
Neutrons interact with… Nucleus
Crystal structure/excitations (eg. phonons)
Unpaired e- via dipole scattering Magnetic structure/excitations (eg. spin waves)
Nuclear scattering Magnetic dipole scattering
Properties of the neutron Mass mn =1.675 x 10-27 kg Charge 0 Spin-1/2, magnetic moment µn = -1.913 µN
NXS School
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Wavelength-energy relations
NXS School 7
Neutron as a wave … Energy (E), velocity (v), wavenumber (k), wavelength (λ)
Energy (meV) Temperature (K) Wavelength (Å)Cold 0.1 – 10 1 – 120 4 – 30Thermal 5 – 100 60 – 1000 1 – 4Hot 100 – 500 1000 – 6000 0.4 – 1
E =h2k 2
2mn
=h2
2mn
2πλ
2
=81.81meV ⋅ Å2
λ2
k =mnvh
=2πλ
E = kBT = 0.08617meV ⋅ K−1( )T
λ ~ interatomic spacing E ~ excitations in condensed matter
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The Basic Experiment:
(θ, φ)
Incident Beam:
• monochromatic• “white”• “pink”
Scattered Beam:
• Resolve its energy• Don’t resolve its energy• Filter its energy
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Fermi’s Golden Rule within the 1st Born Approximation
W = 2π /h |< f | V | i>|2 ρ (Ef)
δσ = W / Φ = (m/2πh2)2 kf / ki |< f | V | i>|2 δΩ
δ2σ /δΩ δEf = kf/ki σcoh/4π N Scoh(Q, ω)
+ kf/ki σincoh/4π N Sincoh(Q, ω)
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σcoh and σincoh
parametrize the strength of the scattering from the nuclei
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Nuclear correlation functions
11
G(r,t) =1N
δ r'−R j ' (0)( )δ r '+r − R j (t)( )jj '∑ dr '∫
Pair correlation function
I(Q,t) = G(r,t)eiQ⋅rdr∫ =1N
exp −iQ ⋅ R j ' (0)( )exp iQ ⋅ R j (t)( )jj '∑
Intermediate function
S(Q,ω) =1
2πhI(Q,t)e− iωtdt∫
Scattering function
d2σdΩdE f
=σ scat
4πk f
ki
NS(Q,ω)
Differential scattering cross-section
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Nuclear (lattice) excitations
NXS School 12
Commonly studied excitations Phonons Librations and vibrations in molecules Diffusion Collective modes in glasses and liquids
Neutron scattering measures simultaneously the wavevector and energy of collective excitations dispersion relation, ω(q)In addition, local excitations can of course be observed
Excitations can tell us about Interatomic potentials & bonding Phase transitions & critical phenomena (soft modes) Fluid dynamics Momentum distributions & superfluids (eg. He) Interactions (eg. electron-phonon coupling)
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Atomic diffusion
NXS School 13
Cocking, J. Phys. C 2, 2047 (1969)..
Liquid Na
Auto-correlation function
r2(t) ≈ 6Dt
For long times compared to the collision time, atom diffuses
Gs(r,t) = 6π r2(t) −3 / 2exp −
r2
6 r2(t)
S(Q,ω) =1
πhexp hω
2kBT
DQ2
ω 2 + (DQ2)2
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Molecular vibrations
NXS School 14
Prassides et al., Nature 354, 462 (1991).C60 molecule
Large molecule, many normal modes Harmonic vibrations can determine interatomic potentials
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2 π / a
2 π / a
Origin of reciprocal space;
Remains fixed for any sample rotation
Crystalline Materials: Structure is Periodic with Period a
Work in Reciprocal Space – Momentum space, most natural for understanding diffraction and scattering
Mapping Momentum – Energy (Q-E) space
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Q
ki
kf
-kf
Bragg diffraction:
Constructive Interference
Q = Reciprocal Lattice Vector
Elastic scattering : | ki | = | kf |
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Q
ki
kf
-kf
Bragg diffraction:
Constructive Interference
Q = Reciprocal Lattice Vector
Elastic scattering : | ki | = | kf |
2 π / a
a
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Q
ki
kf
-kf
Bragg diffraction:
Constructive Interference
Q = Reciprocal Lattice Vector
Elastic scattering : | ki | = | kf |
2 π / a
a
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Elementary Excitations in Solids
• Lattice Vibrations (Phonons)• Spin Fluctuations (Magnons)
Energy vs Momentum
• Forces which bind atoms together in solids
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Phonons
20Lynn, et al., Phys. Rev. B 8, 3493 (1973).
Normal modes in periodic crystal wavevector
Energy of phonon depends on q and polarization
FCC Brillouin zone
FCC structure
u(l,t) =1NM
ε j q( )exp iq⋅ l( ) ˆ B qj,t( )jq∑
Longitudinal modeTransverse mode
NXS School
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Phonon intensities
21Guthoff et al., Phys. Rev. B 47, 2563 (1993).
S1+ Q,ω( )=1
2NMe−Q 2 u2 Q ⋅ ε j q( )
2
ω j q( )1+ n ω( )( )δ Q − q − τ( )δ ω −ω j q( )( )
jq∑
Structure (polarization) factor
0 1/2
Trans
Phon
on E
nerg
yq, [ξ00]
Long
NXS School
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More complicated structures
22
Woods, et al., Phys. Rev. 131, 1025 (1963). Optical phonon
Acoustic phonon
La2CuO4
Chaplot, et al., Phys. Rev. B 52, 7230(1995).NXS School
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Spin excitations
NXS School 23
Spin excitations Spin waves in ordered magnets Paramagnetic & quantum spin fluctuations Crystal-field & spin-orbit excitations
Magnetic inelastic scattering can tell us about Exchange interactions Single-ion and exchange anisotropy (determine Hamiltonian) Phase transitions & critical phenomena Quantum critical scaling of magnetic fluctuations Other electronic energy scales (eg. CF & SO) Interactions (eg. spin-phonon coupling)
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Spin waves
NXS School 24
Perring et al., Phys. Rev. Lett. 77, 711 (1996).
Ferromagnetic
Shapiro et al., Phys. Rev. B 10, 2014 (1974).
Antiferromagnetic
Ferrimagnetic
McQueeney et al., Phys. Rev. Lett. 99, 246401 (2007).
Fe3O4
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25
Scattering experimentsSingle-crystal
Instrument and sample (powder or single-crystal) determine how (Q,ω) space is sampled
Powder S(|Q|,ω)
NXS School
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Kinematic limitations
• Many combinations of ki,kf for same Q,ω– Only certain configurations are used (eg. Ef-fixed)
• Cannot “close triangle” for certain Q,ωdue to kinematics
May 31, 2009 NXS School 26
Kinematic limits, Ei=160 meV
ki
kf
Q
ki kf
Q
Minimum accessible Q
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Bragg’s Law: nλ = 2d sin(θ)
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Bragg’s Law: nλ = 2d sin(θ)
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| ki | = 2 π / λi
| kf | = 2 π / λf
Brockhouse’s Triple Axis Spectrometer
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Momentum Transfer:
Q = ki – kf
kf
- kf
ki
Q
Energy Transfer:
δ E = h2/2m (ki2 – kf
2)
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Two Axis Spectrometer:
• 3-axis with analyser removed
• Powder diffractometer• Small angle diffractometer• Reflectometers
Diffractometers often employ working assumption that all scatteringis elastic.
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Soller Slits: Collimators
Define beam direction to +/- 0.5, 0.75 etc. degrees
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Filters: Remove λ /n from incident or scattered beam, or both
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nλ = 2d sin(θ)
Get: λ , λ/2 , λ/3 , etc.
Single crystal monochromators:
Bragg reflection and harmonic contamination
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Pyrolitic graphite filter:
E = 14.7 meVλ = 2.37 Av = 1.6 km/s2 x v = 3.2 km/s 3 x v = 4.8 km/s
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Bragg’s Law: nλ = 2d sin(θ)
| k | = 2 π / λ
Volume of Q – E space sampled
~ k3 cot (θ)
“Efficiency” of monochromator / analyservaries strongly with k, θ
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Q
ki -kf
Bragg Diffraction:
Two Axis Diffraction: No Ef discrimination
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Constant kf Constant ki
Two different ways of performing constant-Q scans
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Constant kf:
• kf , θA do not change;therefore analyser “efficiency” isconstant
• ki, θM do change, but monitor detector normalizes toincident neutron flux
• Monitor detector (low) efficiencygoes like ~ 1/v ~ 1/ki
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δσ = W / Φ = (m/2πh2)2 kf / ki |< f | V | i>|2 δΩ
δ2σ /δΩ δEf = kf / ki σcoh/4π N Scoh(Q, ω)
Recall that our cross-section was:
Which gave us (keeping only the coherent scattering)
However, we are measuring the incident flux with an efficiency of 1/ki
So, for constant kf, this means we measure:
δ2σ /δΩ δEf = kf/ki σcoh/4π N Scoh(Q, ω) / 1/ki ~ Scoh(Q, ω)
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2 π / a
2 π / a
Origin of reciprocal space;
Remains fixed for any sample rotation
Mapping Momentum – Energy (Q-E) space
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Elementary Excitations in Solids
• Lattice Vibrations (Phonons)• Spin Fluctuations (Magnons)
Energy vs Momentum
• Forces which bind atoms together in solids
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Constant Q, Constant E3-axis technique allow us toPut Q-Energy space on a grid,And scan through as we wish
Map out elementary excitations In Q-energy space (dispersion Surface)
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Inelastic x-ray scattering
• Ei=20 keV, need 1 meV resolution• ∆E/Ei ~ 10-7 !!!
May 31, 2009 NXS School 46
analyzer
Sector-3, APS
φ-scan of monochromator1 meV ⇒ µrad
T-scan of monochromator1 meV ⇒ 0.02 K
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Samples
• Samples need to be BIG– ~ gram or cc– Counting times are long (mins/pt)
• Sample rotation• Sample tilt
May 31, 2009 NXS School 47
HB3-HFIR
IN14-ILL
Co-aligned CaFe2As2 crystals
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Monochromators
• Selects the incident wavevector
• Reflectivity• focusing• high-order contamination
eg. λ/2 PG(004)
l
Q(hkl) =2π
d(hkl)= 2ki sinθθ
Q(hkl)
Mono d(hkl) uses
PG(002) 3.353 General
Be(002) 1.790 High ki
Si(111) 3.135 No λ/2
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Detectors
• Gas Detectors• n + 3He 3H + p + 0.764 MeV• Ionization of gas• e- drift to high voltage anode• High efficiency
• Beam monitors• Low efficiency detectors for
measuring beam flux
NXS School 49
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Resolution
• Resolution ellipsoid– Beam divergences– Collimations/distances– Crystal mosaics/sizes/angles
• Resolution convolutions
NXS School 50
I(Q0,ω0) = S(Q0,ω0)∫ R(Q − Q0,ω −ω0)dQdω
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Resolution focusing
• Optimizing peak intensity• Match slope of resolution to dispersion
May 31, 2009 NXS School 51
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Neutrons have mass so higher energy means faster – lower energy means slower
We can measure a neutron’s energy, wavelength by measuring its speed
v (km/sec) = 3.96 / λ (A)
• 4 A neutrons move at ~ 1 km/sec• DCS: 4 m from sample to detector• It takes 4 msec for elastically
scattered 4 A neutrons to travel 4 m
• msec timing of neutrons is easy• δ E / E ~ 1-3 % - very good !
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Time-of-flight methods
NXS School 53
velocity selector
sample
detector banks
Scatteredneutrons
Spallation neutron source Pharos – Lujan Center
Effectively utilizes time structure of pulsed neutron groups
t =dv
=mh
d
λ
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Fermi Choppers
• Body radius ~ 5 cm• Curved absorbing slats
– B or Gd coated– ~mm slit size
• f = 600 Hz (max)• Acts like shutter, ∆t ~ µs
NXS School 57
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T-zero chopper
• Background suppression• Blocks fast neutron flash
NXS School 58
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Position sensitive detectors
• 3He tubes (usu. 1 meter)• Charge division• Position resolution ~ cm• Time resolution ~ 10 ns
NXS School 59
MAPS detector bank
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Sample environment
• Temperature, field, pressure• Heavy duty for large
sample environment– CCR– He cryostats– SC magnets– …
May 31, 2009 NXS School 60
HB3-HFIR
IN14-ILL
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Guides• Transport beam over long distances• Background reduction• Total external reflection
– Ni coated glass– Ni/Ti multilayers (supermirror)
NXS School 61
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Size matters• Length = resolution
– Instruments ~ 20 – 40 m long– E-resolution ~ 2-4% Ei
• More detectors– SEQUOIA – 1600 tubes, 144000 pixels– Solid angle coverage 1.6 steradians
• Huge data sets• 0.1 – 1 GB
NXS School 62
SEQUOIA detectorvacuum vessel
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63
Data visualization• Large, complex data from spallation sources• Measure S(Q,ω) – 4D function
Ye et al., Phys. Rev. B, 75 144408 (2007).
La1-xCaxMnO3
NXS School
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The appearance of spin waves indicates that the field-induced state is long range ordered
Development of Long Range Order
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Weak magnetic field // [110] induces LRO:
appearance of long-lived spin waves at low T and moderate H
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References
NXS School 66
General neutron scatteringG. Squires, “Intro to theory of thermal neutron scattering”, Dover, 1978.S. Lovesey, “Theory of neutron scattering from condensed matter”, Oxford, 1984.R. Pynn, http://www.mrl.ucsb.edu/~pynn/.
Polarized neutron scatteringMoon, Koehler, Riste, Phys. Rev 181, 920 (1969).
Triple-axis techniquesShirane, Shapiro, Tranquada, “Neutron scattering with a triple-axis spectrometer”, Cambridge, 2002.
Time-of-flight techniquesB. Fultz, http://www.cacr.caltech.edu/projects/danse/ARCS_Book_16x.pdf
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Why map reciprocal space?
Crystallography!Variation of Bragg peak intensities = where the atoms are
Peakshape gives spatialcorrelations (if resolution effects can be negated)
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Kinematics
• Essentially elastic scattering• No kinematic limits
NXS School 68
Q ≈ 2ki sinθ
hω = hc(ki − k f )
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TOF vs. 3-axis
NXS School 69
epithermal (up to 2 eV) Total spectra (esp. powder
samples) Absolute normalization Low-dimensional systems Hardware inflexible Software intensive
High flux of thermal neutrons Focused studies in Q,ω (soft modes,
gaps, etc.) Three-dimensional systems Hardware intensive Software inflexible
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IXS vs. INS• SAMPLE SIZE
• IXS– Simple scattering geometry (ki≈kf)– Resolution function simpler
(most angles fixed, E-scans only)– No spurions
(high-order refs. keV, no incoherent scat.)– Can only do lattice excitations
0 20 40 60 80 1000
50
100
150
200
250
300
0
100
200
300
400
500
600Fe3O4150 K
X-ra
y Cou
nts/
1000
s
Energy Transfer (meV)
X-ray (Ei=21.66 keV) Neutron (Ef=13.7 meV)
Neutron Counts/1000s
-10 0 10 20 30 40 50 60 70 80 90 1000.0
0.1
0.2
0.3
0.4
LA phonon
magnon
(4.4,0,0)Fe3O4
Coun
ts (a
rb. u
nits
)
Energy Transfer (meV)
neutron x-ray
70NXS School
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NXS School 71
Computation
Pb phonons
Fe3O4 spin waves
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The Basic Experiment:
(θ, φ)
Incident Beam:
• monochromatic• “white”• “pink”
Scattered Beam:
• Resolve its energy• Don’t resolve its energy• Filter its energy
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Absolute normalization
• Absolute normalization– Using incoherent scattering
from vanadium– σ/4π = 404 mbarns/Sr
NXS School 73
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Fermi’s Golden Rule within the 1st Born Approximation
W = 2π /h |< f | V | i>|2 ρ (Ef)
δσ = W / Φ = (m/2πh2)2 kf / ki |< f | V | i>|2 δΩ
δ2σ /δΩ δEf = kf/ki σcoh/4π N Scoh(Q, ω)
+ kf/ki σincoh/4π N Sincoh(Q, ω)
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Spin correlation functions
NXS School 75
Scatteringcross-section
Dipoleinteraction
Spin-spincorrelation function
d2σdΩdE f
=k f
ki
12
γr0gF(Q)
2
δαβ − ˆ Q α ˆ Q β( ) eiQ⋅(R j ' −R j )
jj '∑ 1
2πhdte− iωt∫ S j
α (0)S j 'β (t)
αβ∑
d2σdΩdE f inel
=k f
ki
12
γr0gF(Q)
2
δαβ − ˆ Q α ˆ Q β( )1− ehω / kT( )−1 1π (gµB )2 Im χαβ Q,ω( )
αβ∑
The cross-section is proportional to the magnetic susceptibility,i.e. it is the response of the system to spatially & time varying magnetic field
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Paramagnetic scattering
NXS School 76
Single ion scattering
S jαS j '
β = 0 j ≠ j'( )
S jz (0)S j
z (t) = S jz( )2
e−Γt =13
S j( )2e−Γt =
13
S S +1( )e−Γt
Im χ zz 0,ω( ) πhω
=g2S(S +1)µB
2
3kBT1π
ΓΓ2 + hω( )2
McQueeney et al., Phil. Mag. B 81, 675 (2001).
Inverse width, 1/Γ, gives relaxation time Note crystal field excitation
χ0 =Im χ zz 0,ω( )
πhωdω
−∞
∞
∫ =g2S(S +1)µB
2
3kBT
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77
Scattering experimentsSingle-crystal
Instrument and sample (powder or single-crystal) determine how (Q,ω) space is sampled
Powder S(|Q|,ω)
NXS School
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NXS School 78
Triple-axis instruments
High flux isotope reactor - ORNL HB-1A 3-axis spectrometer
kf
ki Hardware flexibility Constant-Q (or E) scans Ideally suited for single-xtals
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Time-of-flight methods
NXS School 79
velocity selector
sample
detector banks
Scatteredneutrons
Spallation neutron source Pharos – Lujan Center
Hardware inflexible Effective for powders Complicated Q,E-scans a
challenge for single-xtals
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INS data
• Intensities as a function of Q and ω
NXS School 80
Lynn, et al., Phys. Rev. B 8, 3493 (1973).
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Scoh (Q,ω) and Sincoh(Q,ω)describe the structure anddynamics of the atoms andmagnetic moments
σcoh and σincoh
parametrize the strength of the scattering from the nuclei or magnetic moments
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Other triple-axis stuff
• Soller Collimators– Define beam divergence– Q,ω resolution function
• Filters– Xtal Sapphire: fast neutron background– Poly Be: low-energy (5 meV) band pass– PG: higher order contamination
• Masks– Beam definition– Background reduction
May 31, 2009 NXS School 82
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PG filter
May 31, 2009 NXS School 83
• Magic numbers– Best filter for rejection of λ/2 contamination– Ef = 13.7, 14.7, 30.5, 41 meV
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Reciprocal space
May 31, 2009 NXS School 84
hω = Ei − E f
Q = k i − k f
FCC Brillouin zone
q = Q − τWavevector in 1st
Brillouin zone
Scattering triangle
Momentum/energy transferred to sample
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Spurions• Bragg – incoherent – Bragg
– Eg. ki – 2kf
• ħω = 41.1 meV • Ef = 13.7 meV
Ei = 54.8 meV4Ef = 54.8 meV
• Incoherent elastic scattering visible from analyzer λ/2
• incoherent – Bragg – Bragg– Sample 2θ in Bragg condition for kf-kf
– Even for inelastic config, weak incoherent from mono
May 31, 2009 NXS School 85
0
0 20 40 60 80 1000
100
200
300
400
500
600
(mHz,S/N)
(40,0.3)(90,1)
(350,4)
(150,2)
Neu
tron
Cou
nts/
1000
s
Energy Transfer (meV)
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Resolution effects
May 31, 2009 NXS School 86
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Introduction to Inelastic Neutron Scattering
Bruce D Gaulin McMaster University
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