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Exchange springs and exchange bias studied with nuclear methods Francisco Miguel Cruz Sim˜ oes de Almeida Instituut voor Kern-en Stralingsfysica May 24, 2011 Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 1 / 25

Preliminary Doctoral Defense of Francisco Almeida

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My private defense for my PhD in Physics in the Catholic University of Leuven in Belgium.

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Page 1: Preliminary Doctoral Defense of Francisco Almeida

Exchange springs and exchange bias studied withnuclear methods

Francisco Miguel Cruz Simoes de Almeida

Instituut voor Kern-en Stralingsfysica

May 24, 2011

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 1 / 25

Page 2: Preliminary Doctoral Defense of Francisco Almeida

Outline

1 Surface spin-flop in an Fe/Cr superlatticeInterlayer couplingSurface spin-flopPolarized Neutron Reflectometry

2 Exchange bias in Fe-Pt heterostructuresExchange biasFe-Pt alloysFePt/FePt3 bilayersOff-stoichiometric Fe-Pt film

3 Exchange bias through ion beam synthesisIon beam synthesisOxygen implanted cobalt

4 Conclusions

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 2 / 25

Page 3: Preliminary Doctoral Defense of Francisco Almeida

Surface spin-flop in an Fe/Cr superlattice

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 3 / 25

Page 4: Preliminary Doctoral Defense of Francisco Almeida

Fe/Cr superlattice

Multilayer consisting of 22 repetitions of an Fe/Cr bilayer structure

Fe layers 40 A thick.

Cr layers 11 A thick.

Fe

Cr

Fe

Cr

Fe

Cr

Fe

Cr

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 4 / 25

Page 5: Preliminary Doctoral Defense of Francisco Almeida

Fe/Cr superlattice

Multilayer consisting of 22 repetitions of an Fe/Cr bilayer structure

Fe layers 40 A thick and antiferromagnetically coupled.

Cr layers 11 A thick.

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 4 / 25

Page 6: Preliminary Doctoral Defense of Francisco Almeida

Interlayer coupling

Coupling between ferromagnetic layers separated by a spacer layer.

Bilinear Biquadratic

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 5 / 25

Page 7: Preliminary Doctoral Defense of Francisco Almeida

Magnetic response of an Fe/Cr superlattice

Easy axis

M/M

s0.0

0.2

0.4

0.6

0.8

1.0

25 mT

250 mT

[001]

[010]

H

a

Hard axis

µ0H (T)

M/M

s

0.0 0.1 0.2 0.3 0.4 0.5 0.6

0.0

0.2

0.4

0.6

0.8

1.0

25 mT

75 mT

[001

][010]

H

b

J. Meersschaut et al., PRB 73, 144428 (2006)

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 6 / 25

Page 8: Preliminary Doctoral Defense of Francisco Almeida

Magnetic response of an Fe/Cr superlattice

Easy axis

M/M

s0.0

0.2

0.4

0.6

0.8

1.0

25 mT

250 mT

[001]

[010]

H

a

Hard axis

µ0H (T)

M/M

s

0.0 0.1 0.2 0.3 0.4 0.5 0.6

0.0

0.2

0.4

0.6

0.8

1.0

25 mT

75 mT

[001

][010]

H

b

J. Meersschaut et al., PRB 73, 144428 (2006)

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 6 / 25

Page 9: Preliminary Doctoral Defense of Francisco Almeida

Surface spin-flop

Transition (H(S)C ) that causes a top spin/layer to switch orientation before the

remaining spins/layers of an antiferromagnet. The irregularity propagates to the

middle of the spin chain, and leads to a bulk spin-flop (H(B)C ).

H(S)C : surface spin-flop field

H(B)C : bulk spin-flop field

How to visualize a surface spin-flop?

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 7 / 25

Page 10: Preliminary Doctoral Defense of Francisco Almeida

Surface spin-flop

Transition (H(S)C ) that causes a top spin/layer to switch orientation before the

remaining spins/layers of an antiferromagnet. The irregularity propagates to the

middle of the spin chain, and leads to a bulk spin-flop (H(B)C ).

H(S)C : surface spin-flop field

H(B)C : bulk spin-flop field

How to visualize a surface spin-flop?

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 7 / 25

Page 11: Preliminary Doctoral Defense of Francisco Almeida

Polarized Neutron Reflectometry

Similar to X-ray reflectometry.

Sensitive to structural periodicity.

Also sensitive to magnetic periodicity.

Experiment performed in the neutron reflectometer at the HelmholtzZentrum, Berlin.

Neutron wavelength λ = 4.66 A.

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 8 / 25

Page 12: Preliminary Doctoral Defense of Francisco Almeida

Polarized Neutron ReflectometryResults

R++

(a.u.)

10

10

10

10

10

-4

-3

-2

-1

0

5.0x10-5

1.0x10-4

1.5x10-4

Γ ( )-2

Å

0 200 400 600 800 1000Depth (Å)

0.00 0.04 0.08 0.12 0.16

QZ (

-1)Å

0 200 400 600 800 1000Depth (Å)

0.00 0.04 0.08 0.12 0.16

QZ (

-1)Å

0 200 400 600 800 1000

Depth (Å)

0.00 0.04 0.08 0.12 0.16

QZ (

-1)Å

0.00 0.04 0.08 0.12 0.16

QZ (

-1)Å

0 200 400 600 800 1000

Depth (Å)

μ H = 600 mT 0 μ H = 200 mT 0 μ H = 61.8 mT 0 μ H = 30 mT 0

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 9 / 25

Page 13: Preliminary Doctoral Defense of Francisco Almeida

Polarized Neutron ReflectometrySpins configuration: surface spin-flop transition

10-4

10-3

10-2

10-1

100

R+

+ (

a.u

.)

0.00 0.04 0.08 0.12 0.16

QZ (

-1)Å

10-4

10-3

10-2

10-1

100

R+

+ (

a.u

.)

10-4

10-3

10-2

10-1

100

R+

+ (

a.u

.)

10-4

10-3

10-2

10-1

100

R+

+ (

a.u

.)

[001

][010] Hμ H = 600 mT 0

μ H = 200 mT 0

μ H = 61.8 mT 0

μ H = 30 mT 0

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 10 / 25

Page 14: Preliminary Doctoral Defense of Francisco Almeida

Exchange bias in Fe-Pt heterostructures

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 11 / 25

Page 15: Preliminary Doctoral Defense of Francisco Almeida

Exchange biasExample of an oxidized cobalt thin film

Effects observed on the hysteresis loop upon field cooling

Loop shift and broadening

Training

-0.3 -0.2 -0.1 0.0 0.1 0.2 0.3

-1.0

-0.5

0.0

0.5

1.0

M/M

S (a

.u.)

0H (T)

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 12 / 25

Page 16: Preliminary Doctoral Defense of Francisco Almeida

Exchange biasExample of an oxidized cobalt thin film

Effects observed on the hysteresis loop upon field cooling

Loop shift and broadening

Training

-0.3 -0.2 -0.1 0.0 0.1 0.2 0.3

-1.0

-0.5

0.0

0.5

1.0 room temperature 10 K

M/M

S (a

.u.)

0H (T)

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 12 / 25

Page 17: Preliminary Doctoral Defense of Francisco Almeida

Exchange biasExample of an oxidized cobalt thin film

Effects observed on the hysteresis loop upon field cooling

Loop shift and broadening

Training

-0.3 -0.2 -0.1 0.0 0.1 0.2 0.3

-1.0

-0.5

0.0

0.5

1.0 room temperature 10 K (first) 10 K (second)

M/M

S (a

.u.)

0H (T)

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 12 / 25

Page 18: Preliminary Doctoral Defense of Francisco Almeida

Exchange biasMotivation

Origin of exchange bias notoriously difficult to identify.I Behavior very varied from system to system.I Many models of limited applicability.I Most applied techniques focus on the ferromagnet.

Looking into the antiferromagnet:I Local information from the antiferromagnet.I Mossbauer spectrometry of 57Fe.

Let us take advantage of Mossbauer spectrometry.

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 13 / 25

Page 19: Preliminary Doctoral Defense of Francisco Almeida

Exchange biasMotivation

Origin of exchange bias notoriously difficult to identify.I Behavior very varied from system to system.I Many models of limited applicability.I Most applied techniques focus on the ferromagnet.

Looking into the antiferromagnet:I Local information from the antiferromagnet.I Mossbauer spectrometry of 57Fe.

Let us take advantage of Mossbauer spectrometry.

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 13 / 25

Page 20: Preliminary Doctoral Defense of Francisco Almeida

Exchange biasMotivation

Origin of exchange bias notoriously difficult to identify.I Behavior very varied from system to system.I Many models of limited applicability.I Most applied techniques focus on the ferromagnet.

Looking into the antiferromagnet:I Local information from the antiferromagnet.I Mossbauer spectrometry of 57Fe.

Let us take advantage of Mossbauer spectrometry.

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 13 / 25

Page 21: Preliminary Doctoral Defense of Francisco Almeida

Fe-Pt alloys

FePt3 ( Antiferromagnetic, L12 )

FePt (d=100 Å)

MgO (110) (substrate)

Au (capping)

FePt (h)357

FePt ( Ferromagnetic, L10 )

(Fe: red spheres, Pt: white spheres)

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 14 / 25

Page 22: Preliminary Doctoral Defense of Francisco Almeida

Fe-Pt alloys

FePt3 ( Antiferromagnetic, L12 )

FePt (d=100 Å)

MgO (110) (substrate)

Au (capping)

FePt (h)357

FePt ( Ferromagnetic, L10 )

(Fe: red spheres, Pt: white spheres)

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 14 / 25

Page 23: Preliminary Doctoral Defense of Francisco Almeida

Magnetism of FePt3

a) T < 160 K: Q1 wave mode, uncompensated (110) surfaceb) T < 100 K: Q2 wave mode, compensated (110) surface

S. Maat et al., PRB 63, 134426 (2001)

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 15 / 25

Page 24: Preliminary Doctoral Defense of Francisco Almeida

FePt/FePt3 (110) bilayersMagnetic response

FePt semi-easy axis FePt hard axis

FePt

H

FePt3

-2.0 -1.0 0.0 1.0 2.0

-1.0

-0.5

0.0

0.5

1.0

M/M

S (

a.u

.)

0H (T)

SSSSSSSSSSSSSSSSSSSSSSSSSSSSSSS

μ

FePt

// HFePt3

-1.0 0.0 1.0

-1.0

-0.5

0.0

0.5

1.0

M/M

S (

a.u

.)

0H (T)

SSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSSS

μ

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 16 / 25

Page 25: Preliminary Doctoral Defense of Francisco Almeida

FePt/FePt3 (110) bilayersExchange bias (100 A FePt/300 A FePt3)

Observed using a dual approach:

Volume magnetization information (magnetometry).

Local information (Mossbauer from the 57FePt3).

-100

0

100

200

300

400 HE

HC

-1.0 -0.5 0.0 0.5 1.0

-1.0

-0.5

0.0

0.5

1.0

M/M

S (

a.u

.)

0H (T)

μ H

,

μ H

(m

T)

00

CE

μ

0 50 100 150 200 250 300

T (K) v (mm/s)

yiel

d (a

.u.)

-1 0 1

630000

640000

650000

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 17 / 25

Page 26: Preliminary Doctoral Defense of Francisco Almeida

FePt/FePt3 (110) bilayersExchange bias (100 A FePt/300 A FePt3)

What we observe:

Very high roughness and/or intermixing.

Spin-flop coupling between the FePt and the FePt3.

-100

0

100

200

300

400 HE

HC

-1.0 -0.5 0.0 0.5 1.0

-1.0

-0.5

0.0

0.5

1.0

M/M

S (

a.u

.)

0H (T)

μ H

,

μ H

(m

T)

00

CE

μ

0 50 100 150 200 250 300

T (K) v (mm/s)

yiel

d (a

.u.)

-1 0 1

630000

640000

650000

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 17 / 25

Page 27: Preliminary Doctoral Defense of Francisco Almeida

Off-stoichiometric Fe-Pt film

What happens if we field cool a mixture of Fe0.33Pt0.67?

0 20 40 60 80 100 120 140

-30

-20

-10

0

0HE (m

T)

T (K)

SSSSSSSSSSSSSSS

v (mm/s)

Yie

ld (

a.u.

)

-5 0 5

615000

620000

625000

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 18 / 25

Page 28: Preliminary Doctoral Defense of Francisco Almeida

Off-stoichiometric Fe-Pt film

What happens if we field cool a mixture of Fe0.33Pt0.67?

0 20 40 60 80 100 120 140

-30

-20

-10

0

0HE (m

T)

T (K)

SSSSSSSSSSSSSSS

v (mm/s)

Y

ield

(a.

u.)

-5 0 5

615000

620000

625000

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 18 / 25

Page 29: Preliminary Doctoral Defense of Francisco Almeida

Exchange bias through ion beam synthesis

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 19 / 25

Page 30: Preliminary Doctoral Defense of Francisco Almeida

Ion beam synthesis

New method for obtaining exchange bias.

I Reactive implantation grows the antiferromagnet inside theferromagnet.

I Extremely granular structure.I Optimal contact surface.I Parametric control (e.g. fluence, energy).

Synthesis of CoxOy through implantation of 16O into Co.I MBE grown, capped cobalt thin films (thicknesses 600 A and 1000 A).

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 20 / 25

Page 31: Preliminary Doctoral Defense of Francisco Almeida

Ion beam synthesis

New method for obtaining exchange bias.I Reactive implantation grows the antiferromagnet inside the

ferromagnet.I Extremely granular structure.I Optimal contact surface.I Parametric control (e.g. fluence, energy).

Synthesis of CoxOy through implantation of 16O into Co.I MBE grown, capped cobalt thin films (thicknesses 600 A and 1000 A).

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 20 / 25

Page 32: Preliminary Doctoral Defense of Francisco Almeida

Ion beam synthesis

New method for obtaining exchange bias.I Reactive implantation grows the antiferromagnet inside the

ferromagnet.I Extremely granular structure.I Optimal contact surface.I Parametric control (e.g. fluence, energy).

Synthesis of CoxOy through implantation of 16O into Co.I MBE grown, capped cobalt thin films (thicknesses 600 A and 1000 A).

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 20 / 25

Page 33: Preliminary Doctoral Defense of Francisco Almeida

Exchange bias in oxygen implanted cobaltExample

Thin cobalt film implanted with 16O (E = 60 keV, Φ = 1016cm−2).

-0.4 -0.2 0.0 0.2 0.4

-1.0

-0.5

0.0

0.5

1.0 b)

M/M

S (a

.u.)

0H (T)

-1.0

-0.5

0.0

0.5

1.0 a)M

/M

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 21 / 25

Page 34: Preliminary Doctoral Defense of Francisco Almeida

ConclusionsSurface spin-flop in an Fe/Cr superlattice

Surface spin flop like transition detected in a biaxial Fe/Crsuperlattice, along the hard axis.

Demonstrated through Polarized Neutron Reflectometry.

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 22 / 25

Page 35: Preliminary Doctoral Defense of Francisco Almeida

ConclusionsExchange bias in Fe-Pt heterostructures

Exchange bias found in FePt/FePt3 bilayers.I FePt easy axis orthogonal to FePt3 easy axis (spin-flop coupling).I Local information extracted from the antiferromagnet via Mossbauer

spectrometry.

Exchange bias detected in a single layer of disorderedoff-stoichiometric Fe-Pt.

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 23 / 25

Page 36: Preliminary Doctoral Defense of Francisco Almeida

ConclusionsExchange bias in O implanted Co thin films

Exchange bias detected in oxygen implanted Co thin films.I New kind of exchange biased system.

F Antiferromagnet is embedded in the ferromagnet.F Heterogeneous effect.

I Requires a fluence of the order of at least Φ = 1016 cm−2.I The effect is sensitive to the fluence as well as the implantation energy.I Post implantation annealing enhances and homogenizes the obtained

effect.

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 24 / 25

Page 37: Preliminary Doctoral Defense of Francisco Almeida

Conclusion

Many new research opportunities regarding these new systems:

I Exchange bias between Fe-Pt alloys presents new challenges.F Evident direction for further research.F Mossbauer techniques give us more flexibility.

I Exchange bias obtained via ion implantation opens a new field ofresearch:

F Principle may be applied to many other systems besides Co/CoO.F Wealth of technological applications (e.g. patterned implantation).F Theoretical challenge: transition from 2D systems (bilayers) to 3D

systems (implanted films, fully granular structures).

Francisco Almeida (IKS) Doctoral dissertation May 24, 2011 25 / 25