XPCS Studies of Antiferromagnetic Domain f f m g m Wall Dynamics in Elemental Chromium

Oleg Shpyrko Department of Physics, University of California San Diego f lf

Crunchy & Squishy Physics

Soft Condensed Matter Squishy Squishy Gels, Colloids Polymers, Fluids Liquid Crystals Membranes Bio-materials Hard Condensed Matter Crunchy Crunchy Metals, Alloys Oxides (Insulators) Semiconductors Ferroelectrics Magnets

XPCS and other spatio-temporal probes

S(q, ) map:
Length Scale [] XPCS is the extension of dynamic light scattering probe (laser PCS) Energy [e E eV]

Freq quency [H Hz]

INS Raman R Brillouin IXS Spin Echo Spin-Echo

Pros:

laser PCS

XPCS

Smaller lengthscales Non-transparent materials Charge, Spin, Chemical and atomic structure sensitivity

Cons:
1 Scattering Vector Q [-1]

Need fully coherent x-ray sources!

XPCS and other spatio-temporal probes

S(q, ) map:
Length Scale []

Freq quency [H Hz]

INS Raman R Brillouin

Energy [e E eV]

IXS Spin Echo Spin-Echo

laser PCS

??? XPCS

Courtesy G. B. Stephenson

1 Scattering Vector Q [-1]

New X-ray Sources (NSLS-II, LCLS) +Faster detectors!

Mesoscale Texture in Strongly Interacting Fermi Systems

Coexistence of multiple phases:
superconducting and AF domains (stripes or checkerboards) in underdoped high-Tc cuprates AF and FM domains in CMR manganites AFM domains with orthogonal orientation of spin- and charge- density waves in Cr p g y
E. Dagotto, T. M. Rice, Science 271, 618 (1996). T. H T Hanaguri et al., N t i t l Nature 430 1001 (2004) 430, (2004).

High-Tc cuprates

What underlies such mesoscopic texture? Is the texture (domain structure) frozen? What are the effects of thermal and quantum fluctuations?

CMR manganites

AFM chromium

P. G. Evans et al., Science (2002)

S. Mori et al., Nature 392, 473 (1998) M. Uehara et al., Nature 399, 560 (1999)

Brief Review - X-ray Speckle, the early years:

Speckle of (001) Cu3Au peak

M. Sutton et al., The Observation of Speckle by Diffraction with Coherent Xrays Nature 352, 608-610 (1991).

Speckle of the Fe3Al (1/2,1/2,1/2)

Grubel et al., ESRF News (1995)

l tti fl ti h i f i disorder. super-lattice reflection showing frozen-in di d b) Zoom of the central region in a) where the speckle structure is obvious.

Binary Alloys:
Cu3Au
Sutton et al., Nature 1991, PRL 2005

Fe3Al

Brauer et al., PRL 1995 Mocuta et al., Science 2002

CoGa, AlLi, AlZn, CoGa AlLi AlZn AlAg

Stadler et al. 2004-7

Equilibrium:

Non-equilibrium:

Quenched Cu3Au
A. Fluerasu et al., Phys. Rev. Lett. 94, 055501 (2005) M. Sutton et al., Opt. Exp. (2003)

Non Equilibrium Non-Equilibrium (aging) XPCS, contd: cont d

CuPd binary alloy:

Ludwig et al., PRB 72, 144201 (2005)

Charge and Spin-ordered systems:

Nb3Se (classic CDW system)
Sutton, Brock, Thorne et al., J. Phys. 2002, PRB 2001

Cr (CDW/SDW Antiferromagnet)
Shpyrko, Isaacs et al., Nature 2007

Charge and Spin-ordered systems:

Ho films (hel cal AFM) f lms (helical FM)
Koning, Goedkoop, PRL 2007

Pr0 5Ca0 5MnO3 (Charge- & Orbital-Order) (Charge Orbital Order) 0.5 0.5
Turner, Hill, Kevan et al., arxiv (?) 2008 Nelson, Hill, Livet et al., PRB 2002

 Studies of antiferromagnets are more challenging th th h ll i than those of ferromagnets ff t Net magnetic moment = 0 Complex relationship between mesoscale phases (spin, charge, lattice) and Spin domains in Cr P. G. Evans, E. D. Isaacs p y physical properties p p How can we study mesoscale dynamics in the bulk?
X-rays: Scanning X-ray Microscopy g y py (slow dynamics) X-ray Photon Correlation Spectroscopy or XPCS (faster)
Charge/spin density wave domains
10 m

et al., Science 295 1042 ( (2002) )

10 m

Coherent x ray x-ray speckle

Spin Density Wave (SDW) in Chromium:

Commensurate SDW (C-SDW) Wave follows periodicity of W f ll i di i f underlying atomic lattice

Incommensurate SDW (IC-SDW) (IC SDW) Modulation period incommensurate with lattice periodicity

For chromium incommensurability parameter is =0.037 at room T yp (period is -1~28 times the lattice constant)

Charge, Spin and Lattice order parameters:

Real R l Space: Spin Density Reciprocal Space: Charge density

Charge Density Wave satellites

Spin Density Wave satellites

Bragg peak

Microscopic Magnetic Domains in Chromium:

[0, 0, 2-2] Charge-density wave satellite

Scanning X-ray Microscopy:

bulk probe (micron-sized (micron sized penetration depth) spin, charge, lattice and chemical sensitivity
10 m

Domain Wall Fluctuations in Antiferromagnets Antif m n ts

Domain Wall

Magnetic domain wall fluctuations in real and reciprocal space:

1 3 2 2 3 1

1
elemental switching bl k l t l it hi block, w/ volume (/2)3,

Real Space:

Momentum Space:

=3-4 nm

transfer of i f f intensity f i from satellites 1 to 2 due to switch

Random Telegraph Noise in Cr (thin films):

Chromium:

Discrete steps in electrical resistivity Slow (1 s -100 s)

5 R/R ~ 10-5

Is this domain h d switching?

R. Michel, M. Weissman, Phys. Rev. B 44, 7413 (1991).

Random Telegraph Noise in other materials:

Ruthenates (Sr2RuO4): Manganites (La Ca M n nit s (L 1-xC xMnO3):

F. Kidwingira, D. J. Van Harlingen et al., Science 314, 1267 (2006)

Chromium:
B. Raquet et al., Phys. Rev. Lett. 84, 4485 (2000)

R. Michel, Phys. Rev. B 44, 7413 (1991)

R. D. Merithew et al., Phys. Rev. Lett. 84, 3442 (2000)

Random Telegraph Noise measurements:

Focus on the Domain Wall

~100 nm

focused x-ray beam ~100 nm (0.5 m)

X-ray Photon Correlation Spectroscopy (XPCS):

10 m

t + 3t t + 2t t t + t

t + 4t

speckle pattern

t + t

t + 2t

t + 3t

t + 4t

O. G. Shpyrko et al., Nature 447, 68 (2007)

CCD camera

r 2 Q=(0,0,2) a

r k'

r k

Control experiment: Bragg Speckle

Quasi-static Brag speckle (line scans from 2D image):

X-ray Bragg speckle (6 hr (6-hr average)

O. G. Shpyrko et al., Nature 447, 68 (2007)

Bragg, 300K: (total 6 hrs) linescans

x 10
6

D : \ b ra g g _ R T _ 1 5 x 4 0 _ 6 h rs \ b ra g g _ R T _ 1 5 x 4 0 _ 6 h rs _ 0 0 0 0 1 -0 7 0 1 0 . im m L in e = 7 5 , F ra m e : 1 -1 4 0 1 F ra m e : 1 4 0 2 -2 8 0 1 F ra m e : 2 8 0 2 -4 2 0 1 F ra m e : 4 2 0 2 -5 6 0 1 F ra m e : 5 6 0 2 -7 0 0 1

CDW, 4K: 6 hrs

x 10 3
6

D:\cdw_4K_15x40_2\cdw_4K_15x40_2_00001-05010.imm Line=70, Frame:1-1001 Frame:1002-2001 Frame:2002-3001 Frame:3002-4001 Frame:4002-5001

2.5 25
0

20

30

40

50

60

70

80

1.5

0.5

20

25

30

35

40

45

50

55

60

65

70

Autocorrelation function g2(t): Multiple relaxation timescales

17K, fit =3000s fit 1 =3300s 2 =40s 1

[g2(t)-1]/A g A

0.8

S2(q,t)/S2(q,0)

0.6

40 s
r r r r r 2 I (Q, t )I (Q, t + ) g2 (Q, t) = 1+ A[S(Q, t) / S(Q)] = r 2 I (Q, )

0.4

0.2

3,000 3 000 s
0 10
1

10

100

10

time [s]
time [s]

1,000

10

10,000

10

Autocorrelation data:
Bragg speckle gg p

O. G. Shpyrko et al., Nature 447, 68 (2007)

Classical Arrhenius model

E (T ) = exp k BT
1 R 1 QM 1 R

Quantum Tunneling model:

S (T ) =

E + exp k BT

O. G. Shpyrko et al., Nature 447, 68 (2007)

Slow Dynamics in Soft Matter

Onion gel
1 .0 0 .8

f f(t,q)

0 .6 0 .4 0 .2 0 .0 -7 10

-relaxation (cage) -relaxation (collective) compressed exponential

10
-5

10

-3

10

-1

10

10

10

t (s e c )

Final relaxation: compressed exponential (q, ) e p[ ( / w . d f(q,t)=exp[-(t/f)] with ~1.5 and f q-1
L. Ramos and L. Cipelletti, Phys. Rev. Lett. 87, 245503 (2001)

Aging of Soft Matter under jamming transition (using Laser speckle PCS)
reviewed in L. Cipelletti et al., Faraday Discuss. 123 (2003)

Colloidal gels
1.00

Micellar polycrystal
0.8

Concentrated Emulsions
1.0 10

0.75

0.50 0.25 0.00 0 10

q (cm ) 249 338 459 618 833 1133 1528 2058 2782 3756 5066 6745

-1

0.6

21 deg 45 deg 80 deg

f(qg (t) - 1 q,t)

f f(q,)

0.4 0.2 0.0 0 10

f(q,t)
10
1

0.5

10

10

10

( (sec) )

10

10

10

C:\lucacip\Origin\DLS CCD\000709_F108_000329B

10 10 t (sec)

10

10

0.0 10
1

10

10

10

t (sec)

f(q,) exp[-(t/f)1.5], f q-1

What does next generation of sources (NSLS II) b i us? (NSLS-II) bring ?
Brightness=Coherent Flux
brightness=1021 Photons/sec/mm2/mrad2/0.1%BW or =Flux/emittance/0.1% BW Ratio of source emittance to diffraction limited emittance 2/4 is coherent fraction

1. Enhanced spatial resolution (for the same temporal 1 E h d i l l i (f h l scale) scales as rmin~1/I 2. Enhanced temporal resolution scales as min~1/I2

Intensity
~2-3 x 10-3 -1

~10-2 -1

Q QBragg

Intensity
~2-3 x 10-3 -1

x30 increase in coherent flux (brightness)

I ~ (Q)-2
~10-2 -1

~5 fold increase in Q (resolution)

~5x10-2 -1

QBragg
Instead of /10-2-1 ~30 nm, resolution becomes ~6 nm

Enhanced time resolution:

For CDW in Cr we could get reasonable statistics at <1 second, possibly d d ibl down t to ~100 ms With x30 factor enhancement in brightness (NSLS-II vs. APS), APS) temporal resolution is improved by a factor x(30)2=1,000 Could get into sub-1 ms regime (in theory need detectors!)
O. G. Shpyrko et al., Nature 447, 68 (2007)

Other Order Parameters:

Magnetic (non-resonant) scattering (non resonant)
For Cr SDW satellite at APS ~ 1 ct/sec (coherent flux) Factor of 30 helps, but realistically need a factor of ~103+ (!)

Orbital Order:

Second Order Phase Transitions:

Order parameter

Nelson, Hill et al., PRB 66, 134412 (2002)

T emperature Pressure, Magnetic field

Chromium Work X-ray Speckle Collaboration: X-ray Speckle

Oleg Shpyrko and Prof. Eric Isaacs (Center for Nanoscale Materials, Argonne and Physics Dpt., University of Chicago) Yejun Feng, Rafael Jaramillo, Jonathan Logan and Clarisse Kim Prof. Prof Thomas Rosenbaum (University of Chicago) Paul Zschack, 33-ID Michael Sprung, 8-ID p g, Suresh Narayanan, 8-ID Alec R. Sandy, 8-ID ( (Advanced Photon Source, Argonne) anc hoton Sourc , rgonn ) Gabriel Aeppli (U. College London)