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1.010
5
ms
1
, the enormously high speed in axial phase
itself shock-heat the plasmas to very high temperatures
with electron and ion temperatures reaching about 100 and
300 eV, respectively,
48
(ii) current sheath speed in radial compression phase:
46
typically 2 to 2.5 times that of the axial speed,
(iii) pinch plasma electron/ion densities:
13, 49
5 10
24
10
26
m
3
,
(iv) pinch plasma electron temperatures:
50, 51
200 eV
2 keV,
(v) ion temperatures of pinch plasmas:
13
300 eV1.5 keV,
(vi) energies of instability accelerated electrons
28, 45
tens
of keV to few hundreds of keV and
(vii) energies of instability accelerated ions
43, 44
tens of
keV to few MeV.
It may also be noted that the DPF is a pulsed plasma
device with all phenomena of interest being transient in
nature. The durations of pinch plasma and energetic par-
ticles in DPF device are of the order of tens of ns to
about hundred or several hundred ns.
27, 30, 52, 53
The extreme
features of the high energy density plasmas (that include
very high densities and temperatures of pinch plasmas
and very high energies and ux of instability accelerated
charged particles combined with their transient nature) in
DPF devices offers a kind of plasma that is very differ-
ent other plasmas conventionally used (typically low tem-
perature plasmas) in plasma-nanoscience for plasma-aided
nanofabrications.
42
2.4. DPF Devices for Material Processing and
Synthesis: Mechanism and Applications
The rst ever application of DPF device for
(i) processing of bulk material was reported by Feugeas
et al.;
54
a wear reduction by a factor of about 20 in
AISI 304 stainless steel was observed after nitrogen ion
implantation,
(ii) processing of thin lm was reported by Rawat et al.;
55
crystallization in amorphous lead zirconate titanate thin
lm was achieved by single shot energetic argon ion expo-
sure, and
(iii) deposition of thin lm, of carbon, was reported by
Kant et al.
56
It may thus be noticed that the materials related work from
DPF device can be classied into two broad categories:
(i) processing of bulk or thin lm target materials, placed
down stream the anode axis, by the complex mix of insta-
bility accelerated energetic ions from the pinch plasma
and the energetic decaying plasma and ionization wave
and shock front propagating in the forward direction if no
aperture assembly is used (however if the aperture assem-
bly is used then the processing is mostly done by energetic
ion beams only) and
(ii) deposition of thin lms of metals or alloys (which can
be xed to the anode top) and their nitrides, carbides and
oxides using inert gases, hydrogen, nitrogen, methane or
oxygen as operating gases.
2.4.1. Processing of Bulk and Thin Films Using
DPF Device
The formation of a hot, dense pinch plasma column, at the
end of radial collapse phase, is followed by the onset of
instabilities
14, 57
which enhance the induced electric eld
locally leading to the acceleration of ions of lling gas
species with very high energies (few keV to about few
MeV) in the forward direction towards the top of the
plasma focus chamber. The instability accelerated ener-
getic ions are one of main components that process the
bulk or thin lm samples that are placed down the anode
stream.
The pulse duration for the nitrogen ion beam emitted
from a 2.3 kJ DPF device (32 jF, 12 kV, 190 kA) was
estimated to be 140 ns by Hassan et al.,
58
who used
energetic nitrogen ions for processing the Ti substrate to
transform its top layer into TiN. Jiaji et al.
59
used a Fara-
day cup to investigate the ions emitted from the hydrogen
operated plasma focus device and deduced ion energies of
H
+
ions to be in the range of about 35 keV to 1.5 MeV.
Following the method reported by Sanchez and Feugeas,
60
they reported that the total number of ions passing through
a 0.5 mm diameter pinhole placed 10 cm above the anode,
with in 35 keV1.5 MeV energy range, is about 1.2910
11
with a mean energy of 124 keV per ion. The ion ux at
5 cm was estimated to be 2.6310
14
ions cm
2
.
Nanosci. Nanotechnol. Lett. 4, 124, 2012 5
High Energy Density Pulsed Plasmas in Plasma Focus Rawat
The pulse duration of energetic ion beam depends on
pinch phase duration of plasma focus device which in
turn depends on the characteristic time (
L
0
C
0
; where
L
0
and C
0
are system inductance and capacitance respec-
tively) of the device. Most plasma focus devices operate
in typical voltage range of 1020 kV and hence the stored
energy of DPF devices is largely dependent on the capaci-
tance of the system. The high energy plasma focus devices
use bigger capacitor bank (1 MJ PF1000 uses 1320 jF
bank)
13
while the lower energy plasma focus devices use
smaller capacitor banks (3 kJ UNU-ICTP
10
and 0.2 kJ
FMPF-1
15
have 30 and 2.4 jF banks respectively). In low
and mid energy plasma focus the energetic ion beam dura-
tion is of the order of several tens to about hundreds of
ns while in bigger plasma focus device it might be sev-
eral hundred ns. The transient nature of energetic ions as
well as that of hot decaying plasma in DPF device causes
the transient processing of the exposed/irradiated sample.
The ion energy range is not affected, signicantly, by the
change in stored energy of the device and found to remain
in several tens of keV to MeV range. The ion energy ux,
on the sample being exposed, however changes with the
storage energy of the DPF device even if the anode top
to sample distance is kept same as the number of ions in
pinch plasma column changes due to the change in the
size (both radius and length) of the pinched plasma col-
umn with the change in the storage energy of the system.
The increase/decrease in capacitance (for DPFs of differ-
ent storage energy) increases/decreases the quarter time
period of the discharge current; and then the anode dimen-
sion has to be suitably increased/decreased to achieve the
maximum compression efciency in the pinch phase by
synchronizing the occurrence of pinch phase (refer Fig. 2)
with current maximum at about the quarter time period
of the discharge pulse. The change in anode dimensions
changes the size of the pinched plasma column, and hence
the number of ions in the pinched plasma column, as
it is well know through X-ray pin hole imaging results
that the radius and length of the pinched plasma col-
umn are approximately one tenth and equal to radius of
the anode, respectively.
61
This basically implies the inten-
sity/degree of processing of the ion irradiated/exposed
samples depends on the storage energy of the DPF due
to changes in the ion pulse duration and ion energy ux.
Sanchez and Feugeas,
60
considering
(i) the geometry and physical characteristics of the ion
beams of a typical mid energy range DPF device,
(ii) the single-ion-solid interaction process and
(iii) the thermal properties of the materials; estimated the
generation of transient heating slopes and heating speeds
as high as 3600 K jm
1
and 40 K ns
1
respectively.
They showed that the maximum temperatures reached the
material evaporation point at the surface layers and the
cooling down process turned out to be fast enough to pro-
duce the complete thermal relaxation of the target in only a
few microseconds after the end of the ion beam incidence.
It may be important to highlight over here that the sam-
ple exposed in DPF devices are bombarded not only by
transient pulse of instability accelerated ions but also by
(i) strong shock wave that moves in front of the part of the
current sheath that moves axially while radial compression
is going on,
(ii) fast moving ionization wave front that is observed
shadowgraphically (refer Fig. 6(c) of a paper by Lee
et al.
62
showing the bubble formation which is an indi-
cation of fast moving ionization wavefront), and
(iii) hot and still relatively dense decaying plasma after
the pinched plasma column is broken by the m = 0
instability.
The DPF device thus offers a very complex mix of high
energy density plasmas, intense shock wave and instabil-
ity accelerated energetic ion beam that transiently process
the material under irradiation in a very complex way and
hence the exact material processing mechanism will be dif-
cult to predict. However, broadly speaking, these intense
transient phenomena with high energy density can cause
strong thermal effect on the exposed material surface due
to extremely high temperature rise rate followed by rapid
quenching which process the exposed material to bring out
the changes in their several physical properties and com-
positional characteristics.
A signicant amount of work has been done to inves-
tigate the effects of the pulsed ion irradiation in DPF
device on various bulk and thin lm materials by vari-
ous research groups across the globe. The effects of argon
ions irradiation on the amorphous lead zirconate titanate,
Sb
2
Te
3
and oriented CdI
2
thin lms have been reported
by Rawat et al.
55, 64, 64
The amorphization of the crystalline
CdS thin lm and bulk Si (c-Si) using the DPF ion irra-
diation were reported by Sagar and Srivastava
65
and Sadiq
et al.,
66
respectively. The DPF device has also been used
for processing of various bulk and thin lms such as: for
diode formation on polyanilene thin lm,
67
to induce phase
change from non-magnetic o-Fe
2
O
3
to magnetic Fe
3
O
4
phase,
68
to enhance the T
c
of superconducting BPSCCO
thick lms,
69
to irradiate American diamond (high purity
zirconia),
70
to implant/irradiate energetic nitrogen ions
from DPF device on various materials such as zirconium,
aluminum, stainless steel, graphite, ZnO, Ti, nickle ferrite
etc.
7179
2.4.2. Deposition of Thin Films Using DPF Device
The DPF device, in addition to its application in processing
of bulk and thin lms, has also been used extensively for
the deposition of thin lms. During the pinch phase of a
plasma focus shot (operation), two key events from the
thin lm deposition point of view occur:
(i) the instability generated high energy ions of ll-
ing/operating gas species accelerate towards the top of the
chamber and bombard the substrate surface and
6 Nanosci. Nanotechnol. Lett. 4, 124, 2012
Rawat High Energy Density Pulsed Plasmas in Plasma Focus
(ii) at the same time instability accelerated relativistic
electrons (which move towards the DPF anode) and the
high energy density pinch plasma interact with the anode
tip material.
A hollow anode (central electrode) is, therefore, conven-
tionally used in DPF device to minimize the ablation of
metal impurities into the pinch plasma to minimize the
cooling of the pinched plasma by radiation losses to max-
imize the thermonuclear neutron yield from deuterium
operated plasma focus device. For the deposition of thin
lms using DPF device, this efcient ablation of anode
top material is rather used as an advantage wherein a solid
anode (or hollow anode tted with solid anode tip) of
the desired material is used to maximize the ablation for
higher deposition rates.
80
The plasma of the ablated anode
material, which may or may not interact with the plasma
of the lling gas species depending on whether the lling
gas species is reactive or inert, moves towards the sub-
strate and is deposited on to it in the form of a thin lm.
A suitable (inert or reactive) operating gas and anode tip
material combination is used for the deposition of various
types of thin lms.
Typically, multiple plasma focus shots are required for
the deposition of thin lm of a suitable thickness. The
instability accelerated energetic ions during any given
plasma focus shot, transiently process the thin lm (in a
way that has been explained in the previous section) that
has already been deposited before that particular shot. In
other words, the plasma focus device provides an ener-
getic ion assisted deposition that leads to high packing
density in the deposited lms and simultaneous process-
ing (by transient heating) of thin lms during deposi-
tion leading to direct synthesis of crystalline thin lms
without any need for post deposition annealing. Due to
these novel features of dense plasma focus device, many
groups have used it for synthesis of various thin lms.
Kant et al. reported the application of it for carbon
56
and
fullerene
81
thin lm deposition. Rawat et al. have suc-
cessfully deposited thin lms of titanium carbide,
82
tita-
nium nitride,
83
titanium dioxide
84
and Fe
85
thin lms.
Many researchers have deposited diamond like carbon thin
lms using plasma focus device.
81, 8689
Other thin lms
that have been successfully deposited using plasma focus
device are that of FeCo,
90
tungsten nitride,
91
aluminium
nitride,
92
silicon carbide,
93
hafnium oxide
94
etc.
The focus of this review paper is the synthesis of
nanophase magnetic materials using DPF devices which
has been achieved by both the above mentioned mecha-
nisms i.e., by the direct deposition of nanophase magnetic
material in the plasma focus facility and by processing
the PLD grown thin lms of magnetic materials. A brief
review of nanophase magnetic materials is given in the
next section.
3. NANOPHASE MAGNETIC MATERIALS
The nanophase magnetic materials can broadly be divided
into three different types:
(i) nano-particle type: used as recording media, magnetic
uid, magnetic medicine and wave absorption materials,
(ii) nano-microcrystal type: such as magnetically hard and
soft microcrystal materials, and
(iii) nano-structured type: which include magnetic thin
lm, multilayer lms and tunnel junctions.
Nanophase magnetic materials have different properties
from the normal magnetic materials because the physi-
cal lengths relating to magnetic characteristics (such as
single magnetic domain, spin diffusion length, domain
wall thickness, exchange coupling length etc.) are about
1100 nm. Interests in the study of these fascinating
properties have been driven by various promising appli-
cations of nanophase magnetic materials; ranging from
ultra-high density magnetic data storage, biosensors, gas
sensor, toner material for high quality colour copier and
printer, new generation electric motor and generator, envi-
ronment friendly refrigerants, biomedicine etc.
95
In addi-
tion, due to their comparable size to biological entities
(such as 10100 jm cells and 20250 nm viruses), possi-
bilities of surface bio-functionalization and motion control
through external magnetic eld, nanophase magnetic mate-
rials will nd applications in bio-medicine and biotech-
nology such as therapeutic drugs, gene and radionuclide
delivery, radiofrequency-induced destruction of cells and
tumors via hyperthermia, and contrast-enhancement agents
for magnetic resonance imaging etc.
96101
3.1. Nanophase Magnetic Materials in Data Storage
In recent decades, the recording areal density in data stor-
age industry has been increasing at a rate of about a factor
of 10 every 10 years. The introduction (by IBM) of disk
read heads based on the magnetoresistive effect
102
and the
giant magnetoresistive effect
103
allowed the areal data den-
sity growth for magnetic disk drives to accelerate to about
60% compound growth rate during 1990s and towards
the end of the 20th century to an even greater rate of
100% (doubling every year). Starting in 2002, as areal den-
sity increase toward 100 Gbit/in
2
with longitudinal mag-
netic recording
104
accompanying with the appearance of
the thermal stability limitation, maintaining this incredible
rate was no longer possible. Today, the technology is mov-
ing towards 1 Tbit/in
2
areal storage density
105
which is the-
oretically available at perpendicular magnetic recording
106
at a more sustainable pace of about 30% and 40% per year.
One of the main reasons for such rapid advances in areal
density is the signicant achievement in the understand-
ing and control of nanoscaled magnetic lms. In order
to continue to achieve this exponential growth in areal
density, some major obstacles in both recording media
and recording head must be overcome. The most severe
Nanosci. Nanotechnol. Lett. 4, 124, 2012 7
High Energy Density Pulsed Plasmas in Plasma Focus Rawat
areal density limitations result from the magnetic relax-
ation (superparamagnetic limit), the separation of head to
medium, the saturation of write head, the sensitivity of
read head and servo tracking bandwidth
The data areal density limitation on the recording media
resulted from super-paramagnetic limit which is well
established when the particle size reaches the critical vol-
ume. There is a certain amount of energy required to ip
a magnetic domain on a disk surface from one orienta-
tion to the other (representing the ip of data bit from 0
to 1). When this amount of energy becomes compara-
ble to the thermal energy (=kT; where k is the Boltzmann
constant and T the temperature) that a domain has at room
temperature, the domains will spontaneously ip orienta-
tion at random. This so called superparamagnetic limit
puts a ceiling on the areal density that could be achieved.
The transition noise of the media is, and will be, the
dominant noise source in the recording systems. This noise
originates mainly from the roughness of the recorded bit
boundaries. This zigzag shape is due to the magnetic
exchange coupling and magnetostatic interactions between
crystalline grains. To reduce this noise the following two
necessary conditions must be satised:
(i) the grain size of the media must be reduced accord-
ingly with the decreasing recorded bit size, and
(ii) the grains must be magnetically isolated.
The later condition requires that the magnetic and crys-
tal grain sizes be similar. However, the thermal stabil-
ity of the recorded information depends on the magnetic
grain size and the uniaxial anisotropy. A rapid decrease
of the magnetic grain size required an increase in mag-
netic anisotropy in order to maintain the thermal stability
of the recorded information. Also, the non-uniform grain
size will drastically reduce the thermal stability of the
recorded bit due to the thermal decay. Therefore, in order
to push the superparamagnetic limit, uniform grain size is
extremely important.
3.2. Magnetic Recording Media
Magnetic recording is the central technology of the infor-
mation storage, which uses the different patterns of mag-
netization on a magnetic recording media (magnetically
coated surface) to store information.
107
Bits can be written
with the magnetization orientation parallel or perpen-
dicular to media plane which are referred as longitudi-
nal magnetic recording (LMR) or perpendicular magnetic
recording (PMR) respectively. One of the most commonly
followed practices, these days, to overcome the super-
paramagnetic limit, to increase thermal stability, is to use
lms of materials, such as CoSm and CoCr, CoPt,
108110
FePt
109112
and CoCrPtM (M=Ta, Nb, B, C, etc.) alloys,
which have higher values of magnetic anisotropy K
u
for
the magnetic recording media. The FePt and CoPt lms
with atomic percentage of 50:50 are believed to be the
most prominent candidates for ultra-high density magnetic
data storage, which requires:
(i) small particle size (critical value is around 3 or 4 nm)
with tight size distribution
(ii) fct phase with high magnetocrystalline anisotropy
and preferred crystal orientation to overcome the super-
paramagnetic limit, and
(iii) reduced exchange coupling effects with well-
separated distribution of nanoparticles.
Therefore, reduction of ordering temperature, control of
the fct-(001) orientation of thin lms and decrease of grain
size are three key challenges for practical application of
L1
0
phase FePt and CoPt thin lms nowadays.
4. NANOPHASE HARD MAGNETIC
MATERIALS USING DPF DEVICE
In this section the synthesis of nanophase hard magnetic
materials of FePt/CoPt using DPF devices with probable
potential applications in ultra-high density magnetic data
storage will be reviewed. As mentioned before the thermal
effects in any system, due to preferably room temperature
operation requirement of devices for economic feasibil-
ity, are unavoidable. There exists a thermal limit, known
as super-paramagnetic limit, where the magnetic energy
stored in the grains becomes comparable to their thermal
energy, making them impossible to store magnetic states.
The relaxation of the magnetization orientation of each
data storage bit is determined by t =t
0
e
K
u
V,2kT
, in which
t is the relaxation time at one orientation, K
u
is the stor-
age medias anisotropy constant, V is the volume of the
storage bit, k is the Boltzmanns constant, and T is tem-
perature. As the size of data storage bit decreases there
comes a point where the magnetic energy K
u
V becomes
comparable to the thermal energy kT and then the mag-
netization of the data bit starts to uctuate from one ori-
entation to another (magnetization reversal) due to short
relaxation time making it impossible to store the magnetic
state. In general, the ratio of the stored magnetic energy
K
u
V to that of the thermal energy kT needs to exceed 40
for the data stability greater than 10 years. Therefore, to
have smaller size of storage bit for higher storage density,
the storage media should be made of materials with higher
anisotropy constant.
The FePt and CoPt binary alloy nanoparticles, contain-
ing a near-equal atomic percentage of Fe/Co and Pt, are
an important class of magnetic nanomaterials as they are
chemical stabile and exhibit the possibility of existing in
a phase with high magnetic anisotropy constant K
u
. As
shown in Figure 3, the FePt is known to have two solid
phases; CoPt also has exact similar solid structures with Fe
simply being replaced by Co. These two phases basically
are in two types of crystal structures:
113
(i) chemically disordered face-centered-cubic (fcc) struc-
tured A1 phase and
8 Nanosci. Nanotechnol. Lett. 4, 124, 2012
Rawat High Energy Density Pulsed Plasmas in Plasma Focus
(a) (b)
Fig. 3. Schematic diagram of the unit cell of (a) chemically disordered
fcc and (b) chemically ordered fct FePt. For CoPt the Fe is simply
replaced by Co.
(ii) chemically ordered face-centered-tetragonal (fct)
structured L1
0
phase.
The FePt and CoPt exhibit a fcc structure with a ran-
dom distribution of Fe/Co and Pt atoms in corner posi-
tions and face centred positions, refer to Figure 3(a). In
this A1 phase, FePt and CoPt have lower anisotropy con-
stant K
u
with smaller coercivity value and exhibit magnet-
ically soft character. The fully ordered fct phase of FePt
or CoPt can be viewed as alternating atomic layers of
Fe/Co and Pt stacked along the (001) direction (c-axis), as
shown in Figure 3(b), which has high anisotropy constant
K
u
with a high coercivity value and thus exhibits mag-
netically hard character. The FePt and CoPt in ordered fct
L1
0
phase are found to have high uniaxial magnetocrys-
talline anisotropy constants of (6.610) 10
7
erg/cm
3
and 4.910
7
erg/cm
3
, respectively.
114
Due to their excep-
tionally high K
u
value these materials can exhibit ferro-
magnetic character up to the nanoparticle size of about
34 nm.
It may, however, be noted that the as-deposited, when
deposited at room temperature, FePt and CoPt show a
disordered fcc structure which is magnetically soft (low
coercivity) and need to undergo a phase transition from
the disordered fcc structured A1 phase to the ordered
fct structured L1
0
phase after post-deposition annealing
at an elevated substrate temperature of about 600 to
700
C to exhibit hard magnetic character required for
data storage.
115
However, the high annealing temperature
needed for the phase transition, which is reported to be
greater than 500
C,
116, 117
may cause nanoparticle agglom-
erations or grain growth and hence the particles may no
longer stay isolated which lead to the deterioration of
magnetic properties and also the increase in particles size
is undesirable for ultra-high data storage density. Hence,
achieving low temperature phase transition in FePt/CoPt
thin lms from magnetically soft low K
u
fcc-structured
A1 phase to magnetically hard high K
u
fct-structured L1
0
phase is one of the key challenges in ultra-high density
magnetic data storage.
4.1. Lower Phase Transition Temperature in PLD
Grown FePt Thins Films Using DPF Device as
Energetic Ion Irradiation Facility
Several methods have been adopted to lower the order-
ing temperature of FePt. The addition of a third element
(Cu, Ag, and Au) into these alloys was reported to be
effective for reducing the ordering temperature.
118, 119
Lin
et al.
120
reported the lowering of the phase transition tem-
perature to 300
C in FePt:Al
2
O
3
nanocomposite thin lms
synthesized by magnetic trapping assisted pulsed laser
deposition. Another approach for lowering down the phase
transition temperature is using ion irradiation.
121, 122
Ion
irradiation has been considered as an effective technique
to lower down phase transition temperature and simul-
taneously tune the structural and magnetic properties of
lms. The mechanism involved in continuous ion beam
irradiation has been discussed by Devolder et al.
123
He
+
irradiation was reported to control the degree of chemical
ordering in FePt/FePd lms.
124, 125
High energy (350 keV)
He
+
irradiation was used by Wiedwald et al. to lower the
ordering temperature of FePt lm by more than 100
C.
126
It was also reported that the ordered L1
0
FePt phase was
directly achieved by using continuous 2 MeV He
+
irradi-
ation for about 1 hour.
127
However, all of these ion irradi-
ation results are obtained by continuous ion sources with,
typically, hours of irradiation duration. In the following
sub-section, the lowering of fcc to fct phase transition
temperature of the PLD grown FePT thin lms using the
pulsed energetic ion beam from DPF device is reviewed.
4.1.1. FePt Thin Films by PLD
The FePt with atomic percentage of 50:50 is found to
have highest anisotropy constant. The inherent advantage
of stoichiometry preservation in pulsed laser deposition
(PLD)
128
made it an appropriate choice for us for the
synthesis of FePt thin lms and FePt based nanocom-
posite thin lms, as compared to other deposition meth-
ods. In PLD, the atomic mobility of ablated species is
dependent on their kinetic energy and thermal energy.
129
These ablated species are generally generated with a
large amount of internal energy and the main paths of
their stabilization are radiative, evaporative and collisional
cooling.
130
The rst two mechanisms are evidently dom-
inant in plume expansion under vacuum and the last one
is present during the diffusive expansion of the plume
into the ambient gas.
131
Hence, in vacuum or very low
ambient gas pressure, the kinetic or thermal energy of
ablated species is high since there is no collision or very
less collisions with ambient gas, thus their surface mobil-
ity is high
132
leading to smooth and uniform thin lm
formation.
133
It was demonstrated through our work
134
that the morphological features of deposited coatings can
in the form of smooth thin lms, nanoparticle agglom-
erates and/or occules-like nanoparticle networks which
Nanosci. Nanotechnol. Lett. 4, 124, 2012 9
High Energy Density Pulsed Plasmas in Plasma Focus Rawat
are essentially governed by the kinetic energy of ablated
species and, in turn, their surface mobility on the substrate
surface, which can be tailored through the deposition con-
ditions, such as ambient gas pressure, laser energy and
target-substrate distance and geometry.
The FePt in smooth thin form and in the forms of
nanoparticle, nanoparticle agglomerates and occules-like
nanoparticle networks were successfully synthesized by
both conventional PLD and backward plume deposition
(BPD).
59, 134, 135
FePt nanoparticles were also synthesized
by thermal annealing to induce nanostructuring of pulsed
laser deposited smooth thin lms. The thermal anneal-
ing induced FePt nanoparticles are well-separated and
uniformly-distributed but their coercivity value is low due
to the short annealing duration.
134
FePt:Al
2
O
3
nanocom-
posite thin lms, which embed FePt nanoparticles inside
non-magnetic matrix material, were successfully synthe-
sized by conventional PLD using two lasers and specially-
shaped target to reduce their exchange coupling effects
and to minimize typical annealing effects of grain growth
and agglomeration.
136
However, a large number of laser
droplets of aluminium oxide, were observed on deposited
nanocomposite thin lms. To reduce the number of laser
droplets, special target-substrate geometry and strong mag-
netic eld were introduced during the PLD deposition
of FePt:Al
2
O
3
nanocomposite thin lms using PLD. This
magnetic trapping assisted PLD not only signicantly
reduced the number of laser droplets but also lowered
down the fcc to fct phase transition temperature from
600
C to signicantly lower value of 300
C.
120
4.1.2. Processing of PLD grown FePt Thin Films in
Plasma Focus Device
The FePt thin lms with two different thicknesses of about
67 and 100 nm were grown on Si(001) substrates at room
temperature by pulsed laser deposition (PLD)
59, 137
in vac-
uum (better than 310
5
mbar). The Continuum Nd:YAG
laser (532 nm, 10 Hz, 10 ns and 80 mJ) was focused
on FePt (50:50 at%; Kurt Lesker, 99.99%) target disc
with energy density of about 1 10
3
J/cm
2
, and sam-
ples were deposited at the target-substrate separation of
3 cm. The FePt thin lms then were irradiated by highly
energetic H
+
ions using UNU/ICPT (United Nation Uni-
versity/International Center for Theoretical Physics) DPF
device
10
whose details are given in Table I. The sam-
ples were placed axially along the anode axis at various
distances from the anode top and were also exposed to
different numbers of plasma focus irradiation shots. The
working gas used is hydrogen, which was kept at a lling
gas pressure of 5 mbar. Full details of the experimental
setup and irradiation procedures can be found in our papers
by Lin et al.
59
and Pan et al.
137, 138
After exposure, the FePt thin lms were heated in
vacuum furnace to various temperatures, at the rate of
60
C/min, and maintained for 1 hour before being
cooled down naturally. The exposed samples were ana-
lyzed before and after annealing for their morphological,
structural and magnetic properties using various character-
ization tools listed in our papers.
137, 138
4.1.3. H
+
Ion Irradiation on 67 nm FePt Thin Film
Using DPF Device
The PLD grown FePt samples were irradiated by hydro-
gen ions from UNU-ICTP DPF device at a distance of
the 5 cm from the anode top.
59
The morphology of as-
deposited sample and samples after ion irradiation is
shown in Figure 4. The as-deposited FePt thin lms, refer
Figure 4(a), were smooth with laser droplets dispersing on
the surface. The morphology of FePt thin lms changed
from that of the smooth uniform lm to lm with uni-
form and isolated nanoparticles, refer Figure 4(b), after a
single DPF shot exposure. The average particle size were
found to be 9.12.3 nm. As the number of ion irradiation
DPF shots were increased to two, the morphology of irra-
diated samples changed to nanoparticle agglomerates of
bigger size of about 51.37.4 nm, as seen in Figure 4(c).
The change in morphology with the increase in number of
exposure shots is because of the increased energy being
imparted by energetic ions from next shot to the nanopar-
ticles created in the rst exposure which causes them to
migrate and form bigger agglomerates to reduce their sur-
face energy.
The X-ray diffraction (XRD) spectra of as deposited,
single shot irradiated and annealed samples are shown in
Figure 5. The as-deposited thin lms exhibited fcc phase
with a broad peak of (111) at about 41
Dt
A
with D = D
0
exp(E
D
,k
B
T
A
), wherein, D
is the diffusion coefcient, k
B
is Boltzmanns constant, t
A
is the annealing time and T
A
is the annealing temperature.
Since the energetic ion irradiation of FePt thin lm sam-
ples is expected to create higher defect concentration in
these samples and hence the activation energy for diffusion
will be lower in irradiated samples leading to phase transi-
tion from low K
u
fcc to high K
u
fct phase at lower anneal-
ing temperature of 400
C.
4.2. Hard Magnetic Nanophase CoPt Thins Film
Synthesis Using DPF Device
In this section, the deposition of nanostructured magnetic
CoPt thin lms at room temperature on Si substrates using
NX2 DPF device operated at sub-kJ storage energy of
about 880 J, which is reported by us in detail in Ref. [143]
is reviewed.
4.2.1. Experimental Conditions of CoPt Thin Films
Synthesis Using NX2 DPF Facility
The conventional central hollow copper anode of NX2
device, shown in Figure 1, was replaced by a high purity
(50:50 at%; Kurt Lesker, 99.99%) solid CoPt tip tted cop-
per anode. The hydrogen was used as the lling gas as
according to Zhang et al.
28
the NX2 device produces high
energy electrons with higher yields for this gas resulting
in most efcient ablation of the anode target material. Two
sets of experiments were done:
143
(i) the gas pressure was changed from 2 to 8 mbar keeping
the other parameters xed, and
(ii) the number of plasma focus deposition shots was
changed from 25 to 200 shots for xed lling gas pressure
of 6 mbar hydrogen, the optimum gas pressure investi-
gated in rst set, to study the effects of the various number
of focus deposition shots.
The distance between the substrate holder and the anode
top was xed at a relatively bigger distance of 25 cm and
the NX2 DPF was operated at the lower charging voltage
of 8 kV, with storage energy of 880 J, for both sets of
depositions.
4.2.2. Nanophase CoPt Thin Films
The morphological features of the nanostructured CoPt
thin lms were found to depend strongly on the lling gas
pressure and the number of DPF deposition shots used.
The SEM images in Figures 11(a)(d), show the mor-
phology of CoPt thin lms samples deposited at different
lling gas pressures using 25 DPF deposition shots. The
SEM image of the sample synthesized at the lling gas
pressure of 2 mbar, Figure 11(a), showed a two layered
structure with the top layer sintering together to form big
island-like structures and a sub layer of some agglomer-
ates between the nanoislands. For 4 mbar deposition, refer
Figure 11(b), only the particle agglomerates with the aver-
age agglomeration size of 356.0 nm were observed and
the island like structures disappeared. With the increase in
lling gas pressure to 6 and 8 mbar average size of these
Nanosci. Nanotechnol. Lett. 4, 124, 2012 15
High Energy Density Pulsed Plasmas in Plasma Focus Rawat
(a) (b)
(c) (d)
Fig. 11. SEM images of nanostructured CoPt thin lms grown using 25 focus shots at hydrogen lling gas pressures of: (ad) 2, 4, 6, and 8 mbar,
respectively. Reprinted with permission from Ref. [143], Z. Y. Pan et al., J. Phys. D: Appl. Phys. 42, 175001 (2009). 2009, IOP Publishing Ltd.
nanoparticles/particle agglomerate was found to decrease,
refer Figures 11(c) and (d), to 15 3.0 and 10 2.0 nm
respectively. The cross-sectional SEM images that thick-
nesses of the samples deposited at 2, 4, 6, and 8 mbar are
estimated to be about 94.0 4.0, 58.0 3.0, 44.0 2.0
and 22.0 1.0 nm, respectively. The lm thickness and
hence the deposition rate is found to decrease with the
increasing lling gas pressure. The reduction of particle
agglomerate size and the decrease in thin lm deposition
rate (lm thickness) with the increasing lling gas pressure
was because:
(i) the focusing efciency decreases with the increase in
lling gas pressure which results in lesser number of
ablated ions from the anode target with lower kinetic ener-
gies, and
(ii) the collision frequency between the ablation ions and
the ambient gas will increase with increasing operating
pressure which causes the ablated ions to lose more energy
during its movement from the anode to the substrate.
The SEM images of CoPt thin lms samples deposited at
6 mbar using different numbers of DPF deposition shots
(25, 50, 100, 150 and 200 shots respectively) showed
that with the increase in the number of deposition shots,
the morphology changes from well separated small sized
nanoparticles (for 25 shot deposition with particle size of
about 15 nm) to nanoparticle agglomerates of increasing
size e.g., the average size of agglomerate is estimated to
be 32.87.0 nm for the sample deposited with 50 shots.
A typical cross-sectional SEM image of 200 shot depo-
sition sample is shown in Figure 12(a). The thicknesses
of as-deposited samples, estimated from cross-sectional
SEM images, are found to be about 44.02.0, 72.54.0,
208.18.0, 294.514.0 and 331.712.0 nm for 25, 50,
100, 150 and 200 shots deposition samples respectively.
The trend of thickness with number of deposition shots
is shown in Figure 12(b). The slope of linear tted curve
revealed that the average deposition rate of CoPt nanopar-
ticle thin lm was about 1.78 nm/shot for NX2 plasma
focus device operating at 880 J at 6 mbar hydrogen ambi-
ence at the substrate distance of 25 cm from the anode
top. This deposition rate is more than 30 times higher as
compared to that of conventional PLD which is found to
be about 0.50 /shot.
144
The cross-sectional image of the
200 shot deposition sample, refer Figure 11(b), shows rel-
atively uniform thickness and ultra-dense crack free lm.
The different morphological features and thickness
observed on the samples deposited by different numbers
of plasma focus shots can be explained on the basis
of following understanding of the processes of deposi-
tion in plasma focus devices. The ablated species ions
(ions of Co and Pt) accelerate upward along the anode
axis and reach the Si substrate surface with some kinetic
energy. On the substrate surface, the impinging ablated
ions/molecules undergo a diffusion process, due to the
16 Nanosci. Nanotechnol. Lett. 4, 124, 2012
Rawat High Energy Density Pulsed Plasmas in Plasma Focus
Fig. 12. (a) Typical SEM cross-section image of CoPt deposited using
200 focus shots at 6 mbar hydrogen at anode top-substrate distance of
25 cm and (b) the deposition layer thickness as a function of the number
of plasma focus deposition shots. Adapted and Reprinted with permission
from Ref. [143], Z. Y. Pan et al., J. Phys. D: Appl. Phys. 42, 175001
(2009). 2009, IOP Publishing Ltd.
surface mobility they have owing to their kinetic energy,
to cluster together to form nanoparticles. The formation of
clusters/nanoparticles is also possible during the gas phase
dynamics. The ablated material moves from anode top to
the substrate through few mbar of ambient gas and thus it
is slowed down due to its interaction with the ambient gas
taking more time to reach the substrate surface (compared
to what it would have taken if it expands in vacuum). The
ablated material thus interacts more among itself leading to
possible cluster/nanoparticle formation during the expan-
sion in gas phase. Most plasma focus based depositions
are multiple shot depositions. When the second deposi-
tion shot is red, a complex mix of high energy ions of
the lling gas species, sufciently hot and dense decay-
ing plasma from the post pinch phase, fast moving ion-
ization wavefront and a strong shockwave will reach the
substrate surface (as in this case no aperture assembly is
used) and transfer their energy to the nanoparticles/clusters
(deposited during the rst shot) and also to the substrate
surface. This provides a transient annealing of the sam-
ple. This transient heating of the sample promotes the dif-
fusion of clusters/nanoparticles on the surface and they
may coalesce together leading to the formation of bigger
size nanoparticles. The ions/clusters/nanoparticles of the
ablated anode material reach afterward which owing to
their own kinetic energies will also promote coalescence.
As more and more deposition shots are red the clus-
ters/nanoparticle size will grow and even the nanoparticle
will start to bind together to form particle-agglomerates.
The average thickness of the deposition will increase with
the increasing number of shots due to the fact that more
and more material is transferred to the sample surface.
The structural analysis of CoPt thin lms deposited
using 25 DPF shots at different hydrogen ambient gas
pressures from 28 mbar showed that all of as deposited
samples were in fcc phase with a broad and weak peak of
(111) plane at about 41
,
refer Figure 15. The intensities of fundamental (111) and
(200) peaks increased continuously, for all samples, as the
annealing temperature was raised from 400 to 700
C indi-
cating that the crystallinity of the samples was increased.
When the annealing temperature was increased to 600
C,
weak fct superlattice peaks of (001), (110), and (201)
appeared clearly as a result of the phase transition to fct
phase. The intensity of superlattice peaks increased sig-
nicantly when the annealing temperature is increased to
700
C, and a clear splitting of fundamental (200) peak
into fundamental (200) and superlattice (002) peaks was
also observed and all fct peaks became narrow and intense
indicating that the samples were converted into a highly
ordered L1
0
phase.
The average crystallite sizes, estimated from diffraction
results and shown in Table II, for all as-deposited sam-
ples were found to be in a very narrow range of 6.1
0.5 nm and did not increase with the increase in num-
ber of shots. This was because all these depositions were
done at a much bigger distance of 25 cm and simple esti-
mates predict that the temperature rise at this distance will
be insignicant to increase the crystallite size. The aver-
age crystallite size increases for the annealed samples at a
faster rate for the sample deposited using bigger number
of plasma focus shots as shown in Table II. It may also be
noted that the average crystallite size at the given anneal-
ing temperature, say 600
C, increases with the increas-
ing number of plasma focus deposition shots. This may
be due to the fact that even though no signicant tran-
sient annealing was done due to the bigger distance of
deposition (which reduces the ion energy density on the
sample surface), the defects were created by energetic ion
18 Nanosci. Nanotechnol. Lett. 4, 124, 2012
Rawat High Energy Density Pulsed Plasmas in Plasma Focus
(e)
(f)
Fig. 15. XRD patterns of CoPt nanostructures synthesized by (a) 25 (b) 50 (c) 100 (d) 150 and (e) 200 plasma focus shots annealed at different
temperature (400, 500, 600 and 700
C), and (f) the average crystallite size variation as a function of the number of plasma focus deposition shots.
Reprinted with permission from Ref. [143], Z. Y. Pan et al., J. Phys. D: Appl. Phys. 42, 175001 (2009). 2009, IOP Publishing Ltd.
Nanosci. Nanotechnol. Lett. 4, 124, 2012 19
High Energy Density Pulsed Plasmas in Plasma Focus Rawat
Table II. The average crystallite sizes of as-deposited CoPt sample and
samples after annealing at different temperatures and synthesized by dif-
ferent numbers of plasma focus deposition shots.
Annealing Temp.
Room 500
C 600
C 700
C
Number of shots (As-deposited) (nm) (nm) (nm) (nm)
25 6.1 8.8 11.7 14.7
50 5.9 9.1 14.2 15.2
100 5.9 10.2 16.4 17.7
150 5.9 10.5 18.2 18.9
200 6.6 10.8 19.9 21.4
bombardment and more the number of shots more will be
the defects on the deposited sample. The increased defect
concentration will lead to greater reduction in the acti-
vation energy for diffusion and hence the annealing pro-
motes more crystallinity in the samples with bigger defect
concentration.
The hysteresis loops of as-deposited nanostructured
CoPt thin lm samples synthesized using 25, 50, 100, 150
and 200 shots, refer Figure 16(a) and/or Table III, show
weak ferromagnetic signal as they were in low K
u
soft
magnetic fcc phase. The total saturation moments of the
Fig. 16. Hysteresis loops of CoPt nanostructures synthesized by different numbers of plasma focus shots (a) before annealing, and after annealing at
(b) 500, (c) 600, and (d) 700
C. Reprinted with permission from Ref. [143], Z. Y. Pan et al., J. Phys. D: Appl. Phys. 42, 175001 (2009). 2009, IOP
Publishing Ltd.
Table III. The coercivity of as-deposited CoPt sample and samples
after annealing at different temperatures and synthesized using different
numbers of plasma focus deposition shots.
Annealing Temp.
Room 500
C 600
C 700
C
Number of shots (As-deposited) (Oe) (Oe) (Oe) (Oe)
25 20 260 726 607
50 73 450 3060 1338
100 50 402 4962 6850
150 66 592 5664 7529
200 64 742 5477 8973
as-deposited samples increased with the increasing number
of deposition shots due to the increase in the thickness
of the deposited sample. The coercivity of the samples
annealed at 500
C annealed samples though remained low
but it increased with the increase in number of DPF shots
because the crystallinity of fcc phase was enhanced due to
annealing even though it was not transformed to fct phase.
After being annealed at 600
C, a very signicant
increase in the coercivity was observed for the most of
the samples, except for sample deposited with 25 shots,
which can be attributed to the start of phase transition from
20 Nanosci. Nanotechnol. Lett. 4, 124, 2012
Rawat High Energy Density Pulsed Plasmas in Plasma Focus
magnetically soft fcc phase to magnetically hard fct phase
at this temperature which was also noticed in the XRD
results shown in Figure 15. A further increase in annealing
temperature to 700
C resulted in extremely high coerciv-
ity, in excess of 6800 Oe for samples deposited using 100
and 150 shots and reaching to about 9000 Oe for 200 shot
deposition sample, due to achievement of highly ordered
fct structure L1
0
phase in these samples.
5. CONCLUSIONS
The paper reviewed the successful application of dense
plasma focus device, a novel pulsed high energy den-
sity plasma source, in plasma nanoscience as an ener-
getic ion irradiation facility for processing of magnetic
thin lms grown by PLD as well as a high deposition
rate source for magnetic thin lm nanostructured magnetic
material synthesis. The DPF device offers a complex mix-
ture of high energy ions of the lling gas species with
energies ranging from few tens of keV to several MeV,
immensely hot and dense decaying plasma from the post
compression phase with plasma temperature of few keV
and plasma density of the order of 10
23
m
3
, fast moving
ionization wavefront with speed in excess 20 cm/js and a
strong shockwave that provides a unique plasma and phys-
ical/chemical environment that is completely unheard of
in any other conventional plasma based deposition or pro-
cessing facility. The results of two key experimental inves-
tigations on the modication of various physical properties
of PLD grown thin lms of FePt and the deposition of
nanostructured CoPt thin lms were reviewed.
The DPF device, due to use of an aperture assembly,
was essentially used as an intense pulsed ion source to
investigate the effects of ion irradiation on the PLD grown
FePt thin lms of two different thickness of about 67 and
100 nm. By adjusting the operation parameters of ion irra-
diation using UNU/ICTP DPF device, the specic ndings
were:
(1) Nanostructuring of PLD synthesized FePt thin lms,
particularly in nanoparticles form, can be successfully
achieved by energetic plasma focus H
+
ion irradiation.
(2) The annealing temperature for phase transition of FePt
thin lms from low K
u
fcc phase to high K
u
fct phase
was successfully reduced to 400
C by plasma focus ion
irradiation from conventionally required 600
C for such
phase transition. It was postulated that the ion irradiation
lower down the activation energy for diffusion by inducing
the vacancy or interstitial point defects and hence lower
down the annealing temperature for phase transition.
(3) The hard magnetic properties were signicantly
enhanced by single shot plasma focus ion irradiation at
lower post deposition annealing temperature of 400
C
resulting in lesser grain growth or agglomeration of
nanopartilces with reduced exchange coupling effect; a
highly desirable trait for application of these nanoparticles
in ultra high density data storage.
The advantage of energetic ion irradiation using the DPF
device is that it can reduce the phase transition temperature
to hard magnetic phase in a single shot ion exposure with
ion pulse duration of the order of about hundred to few
hundred nanoseconds. The use of transient pulsed ener-
getic ions from DPF device, as opposed to that of long
exposure time irradiation from continuous ion sources,
provides a fast and effective way to lower the phase tran-
sition temperature with signicantly enhanced hard mag-
netic properties with lower particle size.
The NX2 plasma focus device, operating in sub-kJ
range, was successfully used to synthesize CoPt nanopar-
ticles thin lm of as small particle size as possible with
narrow size distribution using:
(i) different hydrogen lling gas pressures keeping the
substrate-anode top distance and the number of plasma
focus deposition shots xed at 25 cm and 25 shots respec-
tively and
(ii) using different numbers of plasma focus deposition
shots at xed substrate-anode distance of 25 cm at lling
hydrogen gas pressure of 6 mbar. The specic ndings
were:
(1) The morphological features, such nanostructure for-
mation and their shapes and sizes, showed a strong depen-
dence on the lling gas pressure and the number of plasma
focus deposition shots. A recipe to synthesize well sepa-
rated and narrow-size distributed CoPt nanoparticles was
obtained by tuning the lling gas pressure and the number
of plasma focus deposition shots.
(2) The deposition rate at a deposition distance of 25 cm
and at an optimized gas pressure of 6 mbar was estimated
to be about 1.78 nm/shot which is more than 30 times
higher as compared to that of conventional PLD which
is reported to be about 0.50 /shot. This proves that the
DPF device provides very high deposition rate facility.
This deposition rate can be further enhanced by a factor
of 4 by reducing the distance to half of its current value.
The uniform deposition can be obtained using a rotating
target holder. Hence, in principle, the energetic electron
beam and hot dense plasma based physical evaporation of
the anode target material in DPF device can provide depo-
sition rates two orders of magnitude higher compared to
that of PLD. The DPF deposition has an added advantage
simultaneously processing of the deposited material by a
complex plasma/ion beam/shockwave mixture providing
an environment unavailable in any other device.
(3) The phase transition, from low K
u
fcc structured A1
phase to high K
u
fct structured L1
0
phase, took place
when the annealing temperature was about 600
C result-
ing in signicantly enhanced hard magnetic properties.
For example, very high coercivities of 6850, 7529 and
8973 Oe are achieved on the samples deposited using 100,
150 and 200 focus deposition shots after 700
C annealing.
These samples also had higher ordering degree indicating
that most of fcc phase was transformed to fct phase.
Nanosci. Nanotechnol. Lett. 4, 124, 2012 21
High Energy Density Pulsed Plasmas in Plasma Focus Rawat
To conclude, the dense plasma focus is indeed a novel
high energy density pulsed plasma device with immense
potential for synthesis of nanophase hard magnetic mate-
rials which should further be explored to other potential
hard magnetic materials and possibly for direct room tem-
perature synthesis of high K
u
fct-structured L1
0
phase hard
magnetic phase.
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Received: 13 September 2011. Accepted: 13 December 2011.
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