The multilayers of [MnPd/Co]10have been investigated for the first time. The results indicate that large perpendicular exchange bias field and magnetic anisotropy were found in these samples below the blocking temperature TB~ 240 K. The dependence of exchange bias on the layer thickness has also been studied. The easy axis direction strongly depends on both the Co and MnPd thicknesses
                
              
                                            
                                
            
 
            
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MINISTRY OF ND TRAINING 
HANOI UNIVERSITY OF TECHNOLOGY 
INTERNATIONAL TRAINING INSTITUTE FOR MATERIALS SCIENCE (ITIMS) 
MASTER THESIS OF MATERIALS SCIENCE 
STUDY OF PERPENDICULAR EXCHANGE BIAS 
MECHANISM IN MnPd/Co MULTILAYERS 
NGUYEN HUU DZUNG 
Supervisor: Prof. D.Sc. Nguyen Phu Thuy Hanoi – 2007 EDUCATION A
ii 
HANOI UNIVERSITY OF TECHNOLOGY 
INTERNATIONAL TRAINING INSTITUTE FOR MATERIALS SCIENCE (ITIMS) 
Batch ITIMS – 2005 
Title of MSc Thesis: 
Study of perpendicular exchange bias mechanism 
in MnPd/Co multilayers 
Author: Nguyen Huu Dzung 
Supervisor: Prof. D.Sc. Nguyen Phu Thuy 
Referees: 1. Dr. Nguyen Thang Long 
 2. Dr. Nguyen Phuc Duong 
Abstract 
The multilayers of [MnPd/Co]10 have been investigated for the first time. 
The results indicate that large perpendicular exchange bias field and magnetic 
anisotropy were found in these samples below the blocking temperature TB ~ 
240 K. The dependence of exchange bias on the layer thickness has also been 
studied. The easy axis direction strongly depends on both the Co and MnPd 
thicknesses. The origin of the perpendicular anisotropy was attributed to the 
magneto-elastic effect due to the strained CoPd interfacial alloy forming at 
the interface between the Co and MnPd layers. In order to explain the 
perpendicular exchange bias mechanism, a phenomenological picture was put 
forward in which the fluctuations of the MnPd spins at the interface play an 
important role. Besides, the results show the anomalous effect related to field-
induced anisotropy, i.e. the parallel field cooling enhanced the perpendicular 
anisotropy property instead of the perpendicular one. 
Keywords: Perpendicular exchange bias, perpendicular magnetic anisotropy, 
magnetic thin films, multilayers. 
iii 
TRƯỜNG ĐẠI HỌC BÁCH KHOA HÀ NỘI 
VIỆN ĐÀO TẠO QUỐC TẾ VỀ KHOA HỌC VẬT LIỆU (ITIMS) 
Khóa ITIMS – 2005 
Tiêu đề của luận văn: 
Nghiên cứu cơ chế trao đổi dịch vuông góc 
trong hệ màng mỏng đa lớp MnPd/Co 
Tác giả: Nguyễn Hữu Dũng 
Người hướng dẫn: GS. TSKH. Nguyễn Phú Thùy 
Người phản biện: 1. TS. Nguyễn Thăng Long 
 2. TS. Nguyễn Phúc Dương 
Tóm tắt 
Lần đầu tiên, hệ màng mỏng đa lớp [MnPd/Co]10 đã được nghiên cứu. 
Kết quả cho thấy độ lớn trường trao đổi dịch và năng lượng dị hướng từ 
vuông góc lớn đã thu được ở dưới nhiệt độ blocking TB ~ 240 K. Sự phụ 
thuộc của hiện tượng trao đổi dịch vào chiều dày các lớp cũng đã được xem 
xét. Hướng của trục dễ phụ thuộc mạnh vào chiều dày của cả hai lớp Co và 
MnPd. Nguồn gốc của dị hướng từ vuông góc được gán cho hiệu ứng từ đàn 
hồi do sự hình thành của hợp kim CoPd ở mặt tiếp xúc giữa lớp Co và MnPd. 
Để giải thích cơ chế của hiện tượng trao đổi dịch vuông góc, một mô hình 
hiện tượng luận đã được đề xuất trong đó sự thăng giáng của các spin lớp 
MnPd ở mặt tiếp xúc đóng một vai trò quan trọng. Ngoài ra, hệ màng đa lớp 
còn thể hiện hiệu ứng dị thường liên quan tới dị hướng cảm ứng từ trường, tức 
là, quá trình làm nguội trong từ trường song song với bề mặt màng làm tăng 
cường tính dị hướng vuông góc thay vì từ trường làm nguội vuông góc. 
Từ khóa: Hiện tượng trao đổi dịch vuông góc, dị hướng từ vuông góc, hệ 
màng mỏng đa lớp MnPd/Co. 
iv 
ACKNOWLEDGEMENTS 
First and foremost, I thank my supervisor Prof. D.Sc. Nguyen Phu Thuy 
for the guidance and inspiration over the last one year at the ITIMS. I would 
like to thank him for his invaluable advice, comments and suggestions. 
I would like to express most sincerely my gratitude to Dr. Nguyen Anh 
Tuan as my co-supervisor at the ITIMS. I would like to thank him for his 
guidance and valuable discussions. 
I also wish to extend my warmest thanks to Dr. Nguyen Thang Long for 
his useful discussions and also for MFM and AFM measurements at the 
College of Technology, Vietnam National University, Hanoi; to Dr. Nguyen 
Phuc Duong for reading my thesis and his feedback; to Dr. Nguyen Nguyen 
Phuoc for many discussions and frank advice; to M.Sc. Do Hung Manh for 
cross-section images and composition analysis at the Institute of Materials 
Science, Vietnamese Academy of Science and Technology. 
Besides, I also wish to extend my thank to Prof. D.Sc. Than Duc Hien for 
the encouragement and the financial support from State Program on 
Fundamental Research. 
Thanks are further extended to all members at the ITIMS for their 
encouragement and kind supports throughout the present thesis. Especially, I 
thank M.Sc. Le Thanh Hung for his useful help in experiments. 
Finally, I would like to thank my family and my friends for their love and 
encouragement during this study. 
October 2007 
 _________________ 
 Nguyen Huu Dzung 
v 
LIST OF NOTATIONS 
θ Angle between incident X-ray and crystal plane (hkl) 
AF Antiferromagnet(s)/ Antiferromagnetic 
AFM Atomic force microscope 
at.% Atomic percent 
EDS Energy dispersive spectrometer 
FC Field cooling 
fct Face centered tetragonal structure 
FESEM Field emission scanning electron microscope 
FM Ferromagnet(s)/ Ferromagnetic 
hcp Hexagonally close packed structure 
H External magnetic field 
HC Coercitive force (Coercitivity) 
HE Exchange bias field 
HFC Cooling field 
JK Unidirectional anisotropy (exchange bias coupling) 
energy 
Keff Effective magnetic anisotropy 
KS Surface/interfacial anisotropy 
KU Uniaxial magnetic anisotropy energy 
KV Volume anisotropy 
M Magnetization 
MFM Magnetic force microscope 
MS Saturation magnetization of ferromagnetic layer 
RF Radio frequency 
SEM Scanning electron microscope 
vi 
T Measurement temperature 
TB Blocking temperature 
TC Curie temperature 
tCo Ferromagnetic layer thickness 
tMnPd Antiferromagnetic layer thickness 
TN Néel temperature 
VSM Vibrating sample magnetometer 
WDS Wavelength dispersive spectrometer 
XRD X-ray diffraction 
ZFC Zero field cooling 
vii 
LIST OF FIGURES 
Fig. 1-1. Schematic diagram of the spin configuration of an 
FM/AF bilayer at different states (After [20]). 5 
Fig. 1-2. Schematic diagram of the spin structures assumed in 
some of the proposed models within each category. 10 
Fig. 1-3. Schematic view of spin configuration of FePt/FeMn 
multilayer based on modified Malozemoff model (After 
N.N. Phuoc et al. [59]). 14 
Fig. 2-1. Schematic view of the MnPd target used in the present 
thesis. 15 
Fig. 2-2. Schematic view of [MnPd/Co]N multilayer structure 
used in the present thesis. 17 
Fig. 2-3. Schematic diagram of glancing incident θ/2θ scan X-
ray diffraction configuration. 18 
Fig. 3-1. X-ray diffraction spectra of [MnPd(10 nm)/Co(x nm)]10 
multilayers, (a) x = 2.5 nm, (b) x = 3.5 nm, (c) x = 4.5 
nm. 24 
Fig. 3-2. Cross-sectional view of [MnPd(10 nm)/Co(7.5 nm)]10 
as-deposited multilayer. 25 
Fig. 3-3. MFM image of [MnPd(10 nm)/Co(3.5 nm)]10 as-
deposited multilayer. 26 
Fig. 3-4. Schematic diagram of measurement configurations for 
samples at 120K. Here, the measurement field direction 
(H) is the same as the cooling field (HFC). 27 
viii 
Fig. 3-5. Parallel and perpendicular hysteresis loops measured at 
T = 120 K for [MnPd(10 nm)/Co(x nm)]10 (x = 2.5, 3.5, 
4.5, 5.5, 7.5, 10 nm) multilayers. 28 
Fig. 3-6. Parallel and perpendicular hysteresis loops measured at 
T = 120 K for [MnPd(y nm)/Co(3.5 nm)]10 (y = 3.5, 5.5, 
7.5, 10, 15.5, 30 nm) multilayers. 29 
Fig. 3-7. Schematic diagram of measurement configurations at 
room temperature. Here, HFC denotes the cooling field 
direction and H denotes measurement field directions. 
Note that all samples were measured in two different 
directions. 31 
Fig. 3-8. Parallel and perpendicular hysteresis loops measured at 
room temperature for [MnPd(10 nm)/Co(x nm)]10 (x = 
2.5, 3.5, 4.5, 5.5, 7.5, 10 nm) multilayers cooled in the 
field perpendicular to the plane. 32 
Fig. 3-9. Parallel and perpendicular hysteresis loops measured at 
room temperature for [MnPd(10 nm)/Co (x nm)]10 (x = 
2.5, 3.5, 4.5, 5.5, 7.5, 10 nm) multilayers cooled in the 
field parallel to the plane. 33 
Fig. 3-10. Parallel and perpendicular hysteresis loops measured at 
room temperature for [MnPd(10 nm)/Co(x nm)]10 (x = 
2.5, 3.5, 4.5, 5.5, 7.5, 10 nm) multilayers cooled in the 
zero field. 34 
Fig. 3-11. Parallel and perpendicular hysteresis loops measured at 
room temperature for [MnPd(10 nm)/Co(x nm)]10 (x = 
2.5, 3.5, 4.5, 5.5, 7.5, 10 nm) as-deposited multilayers. 35 
ix 
Fig. 3-12. Magnetization – temperature curve of [MnPd(10 
nm)/Co(3.5 nm)]10 multilayer in the presence of a field 
of 2500 Oe. 36 
Fig. 4-1. The Co thickness dependence of perpendicular and 
parallel exchange bias fields (HE), coercitivity (HC), 
unidirectional anisotropy constant (JK). 40 
Fig. 4-2. The MnPd thickness dependence of perpendicular and 
parallel exchange bias fields (HE), coercitivity (HC). 42 
Fig. 4-3. (a) The plot of the product of Keff and tCo versus tCo and 
(b) the plot of KU versus tCo of [MnPd(10 nm)/Co(x 
nm)]10 (x = 2.5, 3.5, 4.5, 5.5, 7.5, 10 nm) multilayers at 
120K. 45 
Fig. 4-4. Anisotropy energies of [MnPd/Co]10 multilayers which 
were treated at different conditions. (a) Plot of the 
product of Keff and tCo versus tCo and (b) plot of KU 
versus tCo at room temperature. 47 
Fig. 4-5. Schematic diagram of multilayer structure after 
annealing. 49 
Fig. 4-6. Schematic view of spin configurations of MnPd/Co 
multilayer: (a) perpendicular-to-the-plane easy axis and 
(b) parallel-to-the-plane easy axis. 54 
x 
CONTENTS 
Preface 1 
Chapter 1 Introduction 
1.1 Background 3 
1.2 Overview on exchange bias 6 
1.3 Previous studies on perpendicular exchange bias 12 
Chapter 2 Experimental 
2.1 Introduction 15 
2.2 Sample preparation 15 
2.3 Experimental techniques 18 
2.3.1 Glancing incident X-ray diffraction 18 
2.3.2 Field emission scanning electron microscope 18 
2.3.3 Stylus-method profilemetry 19 
2.3.4 Energy dispersive X-ray spectrometer 19 
2.3.5 Wavelength dispersive X-ray spectrometer 20 
2.3.6 Magnetization hysteresis loops 21 
2.3.7 Magnetization – temperature curve 22 
2.3.8 Magnetic force microscope & atomic force microscope 22 
Chapter 3 Experimental results 
3.1 Introduction 23 
3.2 Crystallographic structure 23 
3.2.1 Glancing incident X-ray diffraction 23 
3.2.2 Cross-section observation 25 
3.3 Magnetic properties 25 
xi 
3.3.1 Domain observation 26 
3.3.2 Magnetization hysteresis loops at low temperature 26 
3.3.3 Magnetization hysteresis loops at room temperature 30 
3.3.4 Temperature dependence of magnetization in MnPd/Co 
multilayers 36 
Chapter 4 Discussions 
4.1 Introduction 37 
4.2 Crystallographic structure 37 
4.2.1 Glancing incident X-ray diffraction 37 
4.2.2 Cross-section observation 38 
4.3 Magnetic properties 38 
4.3.1 Domain observation 39 
4.3.2 Thickness dependence of exchange bias 39 
4.3.2.1 Co thickness dependence of exchange bias 39 
4.3.2.2 MnPd thickness dependence of exchange bias 41 
4.3.3 Perpendicular magnetic anisotropy in MnPd/Co 
multilayers 43 
4.3.3.1. Perpendicular anisotropy at low temperature 44 
4.3.3.2. Perpendicular anisotropy at room temperature 46 
4.3.3.3. Effect of annealing on perpendicular anisotropy 46 
4.3.3.4. Anomalous field induced anisotropy 50 
4.3.4 Temperature dependence of magnetization in MnPd/Co 
multilayers 51 
4.4 Explanation of exchange bias coupling mechanism 52 
Conclusions and further direction 56 
References 58
- 1 - 
PREFACE 
Exchange bias has been studied extensively for over half of a century but 
most of the research has been carried out in the configuration called parallel 
exchange bias. In this configuration, the cooling field and the measurement 
field are applied in the plane. Beside parallel exchange bias, there has been 
very little work carried out in the perpendicular configuration with the cooling 
field and the measurement field along the film normal. Perpendicular 
exchange bias is recently of renewed interest because it is relevant in the 
quest for a better understanding of the microscopic origin of the exchange 
bias phenomenon and it might lead to wide applications in magnetic sensors, 
perpendicular recording media, perpendicular magnetic read heads and also 
magnetic random access memories (MRAMs). 
In this thesis, the studies on perpendicular exchange bias in [MnPd/Co]10 
multilayers are reported for the first time. Since the objective of the present 
thesis is to study the perpendicular exchange bias mechanism, the approach is 
to investigate both the parallel and perpendicular exchange biases. Besides, 
perpendicular anisotropy of the samples at low and room temperatures is also 
investigated due to its important contribution to the effect. 
The present thesis consists of 4 chapters. 
Chapter 1 is to give an overview on exchange bias in both theoretical and 
experimental research; and also previous studies on perpendicular exchange 
bias. 
Chapter 2 focuses on the sample preparation and experimental 
techniques. Some descriptions on the apparatuses and measurements that were 
used in the present thesis are introduced. 
- 2 - 
Chapter 3 represents the experimental results. The aim and configurations 
of measurements and also sample processing procedures are given. 
Chapter 4 is to discuss the results of crystallographic and magnetic 
properties of [MnPd/Co]10 multilayers. The behavior of exchange bias in both 
the parallel and perpendicular directions will be summarized. After that, based 
on that result and the magnetic anisotropy behavior of the samples, we try to 
give a phenomenological picture to explain the perpendicular exchange bias 
coupling mechanism. 
Finally, conclusions and further direction as well as the list of references 
are given at the end of the thesis. 
- 3 - 
Chapter 1 
1. INTRODUCTION 
1.1 Background 
Nowadays, magnetic materials play an important role in the information 
technology oriented social. There are various applications using magnetic 
materials such as magnetic recordings, magnetic sensors, magnetic heads, and 
electronic motors. It is of particular interest to note that through rapid 
technological developments in recent years, thin films and multilayers have 
received much attention. 
Among studies on magnetic materials, the exchange bias coupling between 
ferromagnetic (FM) and (AF) materials is of great interest. Since discovered 
in 1956 by Meiklejohn and Bean [1], there have been many studies published 
in the literature on this effect because of various applications such as spin 
valves, magnetic read heads, magnetic random access memories (MRAMs). 
Although it has been studied extensively, physical origin of this effect is still 
in controversy. 
Exchange bias effect is a phenomenon observed in a system consisting of 
antiferromagnetic and ferromagnetic materials, in which the magnetization 
hysteresis loop is shifted along the field axis after the sample undergoing the 
so-called field cooling process through the Néel temperature of the 
antiferromagnetic material. In other words, its characteristic signature is the 
shift of the center of the hysteresis loop from its normal position at H = 0 to 
HE. However, in order to compare different types of exchange bias systems 
often rather than using the loop shift itself, the so-called unidirectional 
anisotropy energy or exchange bias coupling energy JK = HEMStFM (where MS 
- 4 - 
is the saturation magnetization and tFM is the thickness of the FM layer) is 
evaluated instead. The exchange bias effect is only observed below a certain 
temperature. The temperature at which the exchange bias field becomes zero, 
HE = 0, is usually denoted as blocking temperature (TB). 
Exchange bias can be qualitatively understood by assuming an exchange 
interaction at the AF-FM interface (Fig 1-1). When a field is applied in the 
temperature range TN < T < TC, the FM spins line up with the field, while the 
AF spins remain random (see Fig 1-1-(a)). When cooling to T < TN, in the 
presence of the field (so-called cooling field which is denoted as HFC in 
present thesis), due to the interaction at the interface, the AF spins next to the 
FM align ferromagnetically to those of the FM (assuming that the interaction 
is ferromagnetic). The other spin planes in the AF follow the AF order so as 
to produce zero net magnetization (see Fig 1-1-(b)). When the field is 
reversed, the FM spins start to rotate. However, the AF spins remain 
unchanged due to its large anisotropy. Therefore, the interfacial interaction 
between the AF-FM spins try to align parallel the FM spins. In other words, 
the AF spins exert a microscopic torque on the FM spins, to keep them to 
their original position (see Fig 1-1-(c)). The field needed to reverse 
completely the FM spins is larger if it is in contact with the AF because an 
extra field is to overcome a microscopic torque. As the field is back to its 
original direction, the FM spins will start to rotate back at a smaller field 
because it now exerts a torque with the same direction as the applied field (see 
Fig. 1-1-(d) and Fig 1-1-(e)). The material behaves as if there is an extra 
biased field; the hysteresis loop is therefore shifted along the field axis (see 
the hysteresis loop in Fig 1-1). If the AF anisotropy is large, one should only 
observe a shift of the hysteresis loop, while for small AF anisotropies, the 
only observed effect should be a coercivity enhancement (without any loop 
- 5 - 
FM 
AF 
FM 
AF 
(d) 
(c) (b) 
(a) 
HFC
Field cooling 
H
M
O
HE
Fig. 1-1. Schematic diagram of the spin configuration of an FM/AF 
bilayer at different states. (After [20]) 
FM 
AF 
FM 
AF 
(e) 
FM 
AF 
- 6 - 
shift). Nevertheless, in general, both the effects can be observed 
simultaneously, due to, for example, structural defects or grain size 
distribution, which bring about local variations of the AF anisotropy. 
Although this simple phenomenological model gives an intuitive picture, it 
fails to quantitatively understand of these phenomena. In particular, the 
theoretically predicted exchange bias field is much larger than the 
experimental value. In an attempt to reduce this discrepancy, many models 
such as planar domain wall model [2], random-field model [3-5], spin flop 
model [6] put forward. However, there have not been experimental 
confirmations of these models and they are therefore in controversy. It is due 
to the fact that the role of the many different parameters involved in exchange 
bias, such as anisotropy, interface roughness, spin configuration or magnetic 
domain is far from being understood. A clear understanding of exchange bias 
at the microscopic level is still lacking. Therefore, from the fundamental point 
of view, the subject of exchange bias is still a hot topic for the years to come 
and it is of great interest to study this phenomenon together with its associated 
effects for a better understanding of physical origin. 
1.2 Overview on exchange bias 
So far, exchange bias has been investigated extensively both 
experimentally and theoretically. 
Regarding experimental research, from a view point of material form, 
studies on exchange bias can be relatively divided into 3 categories: exchange 
bias in particles, exchange bias in nanostructures and exchange bias in 
(continuous) thin films. 
Fine particles were the first type of system where exchange bias was 
reported. Since its discovery, exchange bias in particles has been concentrated 
on a number of materials, mainly ferromagnetic metals covered by their 
- 7 - 
antiferromagnetic oxides, such as Co/CoO [1, 7, 8], Ni/NiO [9], Fe/FeO [10], 
Fe/Fe2O3 [11], Fe/Fe3O4 [12]. Recently, the number of studies on exchange 
bias in small particles has been reduced because most of the applications 
using this effect ar