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Smoothing, roughening and sputtering: the complex evolution of immiscible Fe/Bi bilayer

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2008 J. Phys. D: Appl. Phys. 41 215306

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IOP PUBLISHING JOURNAL OF PHYSICS D: APPLIED PHYSICS
J. Phys. D: Appl. Phys. 41 (2008) 215306 (8pp) doi:10.1088/0022-3727/41/21/215306

Smoothing, roughening and sputtering:

the complex evolution of immiscible Fe/Bi
bilayer system
A Gupta1 , R S Chauhan1 , D C Agarwal1 , S Kumar2 , S A Khan3 ,
A Tripathi3 , D Kabiraj3 , S Mohapatra3 , T Som4 and D K Avasthi3
1
Department of Physics, RBS College, Agra 282 002, India
2
Department of ASH (Physics), CITM, Aravali Hills, Sector-43, Faridabad 121 001, India
3
Inter-University Accelerator Centre, Post Box-10502, New Delhi 110 067, India
4
Institute of Physics, Sachivalaya Marg, Bhubaneswar 751 005, India
E-mail: abhiphys@gmail.com

Received 1 June 2008, in final form 7 August 2008

Published 13 October 2008
Online at stacks.iop.org/JPhysD/41/215306

Abstract
In this work, swift heavy ion (SHI) induced surface smoothing, roughening and sputtering of
thermally immiscible Fe/Bi bilayer system has been investigated. The pristine and irradiated
samples were analysed by Rutherford backscattering spectrometry (RBS), grazing angle x-ray
diffraction (XRD), atomic force microscopy and scanning electron microscopy including x-ray
dispersive energy analyzer. RBS analysis revealed that steepness of the low energy edge of the
Bi signal increases at a fluence of 3 × 1013 ions cm−2 , beyond which the slope of the rear edge
decreases. The increased steepness is due to smoothing induced at initial fluence; however, the
decrease in the slope of rear edge beyond 3 × 1013 ions cm−2 fluence is a result of surface
roughening. XRD reveals the increase in the crystalline nature of Bi after irradiation at
3 × 1013 ions cm−2 . Irradiation at higher fluences from 6 × 1013 to 1 × 1014 ions cm−2 leads to
a decrease in the crystalline nature of Bi. Surface roughness of pristine and irradiated samples
from AFM analysis revealed that initially roughness decreases with a fluence of
3 × 1013 ions cm−2 . However, at higher fluences, beyond 3 × 1013 ions cm−2 , the
agglomeration of smaller grains has been observed due to the shear flow mechanism, which
results in surface roughening. The observed behaviour of surface smoothing and roughening
under SHI irradiation may be explained on the basis of the thermal spike model.
(Some figures in this article are in colour only in the electronic version)

1. Introduction immiscible binary metal systems characterized by a large

The formation of non-equilibrium solid phases, including
amorphous and metastable crystalline phases, in binary metal
systems with negative heat of mixing (
Hmix < 0) by ion
beam mixing (IBM) and solid state reaction of multiple metal
layers, has been extensively studied over the last two decades
by experiments as well as by theoretical approaches based
on the thermodynamics of solid and growth kinetics [1–7].
In contrast, the formation mechanism of various metastable
phases in the system with positive heat of mixing (
Hmix > 0)
has not been thoroughly studied and is not yet well understood
[8–11]. The unusual alloying behaviour in these equilibrium
positive heat of mixing has therefore attracted much attention
in recent years by employing some non-equlibrium processing
techniques [12–15]. IBM has been extensively used to form
various metastable phases with either an amorphous or a
crystalline structure in some binary metal systems with a
positive heat of mixing. It has been proved that IBM is
a powerful tool to produce non-equilibrium solid phases,
since an effective cooling speed as high as 1013 –1014 K s−1
is involved in the process [16].
Due to the unique properties of bismuth, such as low
melting point, low toxicity, large Fermi wavelength (40 nm)
[17] and higher carrier mean free path (can be as long as a

0022-3727/08/215306+08$30.00 1 © 2008 IOP Publishing Ltd Printed in the UK

J. Phys. D: Appl. Phys. 41 (2008) 215306
few millimetres at 4.2 K), bismuth and its alloys are widely
used in many industries such as microwave engineering,
medications, thermoelectric generators and refrigerators and
free detection and suppression system safety devices. It has
been reported that at room temperature (RT), the immiscible
Fe/Bi system, characterized by a large positive heat of mixing
(+17.46 kJ mol−1 ), has shown unique physical properties in
some respects, due to its long magnetic relaxation time [18].
This unique characteristic is attributed to the large spin–orbital
splitting of Bi, which prevents the magnetic element from
rapidly releasing its magnetic energy to the system. Honda and
Nagata [19] recently discovered an enhanced Hall coefficient
of 5.25 × 10−10  cm G−1 in the Co–Bi film, which exceeds
that of bulk Co by two orders of magnitude. Hence, the
combination of magnetic metal and semi-metallic Bi gives
rise to numerous peculiar and interesting results. The Fe/Bi
system exhibits complete immiscibility in the condensed state
as shown in the binary phase diagram of Bi/Fe [20]. This
means that a uniform Fe/Bi alloy cannot be formed by solid
diffusion or liquid melt quenching techniques. In principle,
one can fabricate such an alloy by means of non-equilibrium
techniques such as IBM and vapour quenching [21]. To the
best of our knowledge, the immiscible Fe/Bi bilayer system
has not been studied previously by swift heavy ions (SHIs).
Therefore, it is of interest to investigate the possibility of
SHI induced mixing in the immiscible bilayer system. SHI
induced mixing is shown to be a consequence of interdiffusion
during the transient molten phase [22]. Thus, it would be
further interesting to perform the IBM experiment on the Fe/Bi
system, where Fe and Bi both go to the transient molten state
as predicted by the thermal spike model.
A SHI, while traversing through the solid, loses its energy
in two ways: electronic energy loss (Se ) due to inelastic
collision of an energetic projectile ion with electron of the solid
and nuclear energy loss (Sn ) due to elastic collisions with atoms
of the solid. In the MeV energy regime, electronic energy loss
dominates over nuclear energy loss. In such cases, a trail of
defects or amorphous phase is induced along the ion trajectory,
called latent track, when Se exceeds a threshold value of
‘Seth ’. It may be mentioned that under the present conditions,
the contribution of electronic energy loss of 20 keV nm−1
and 34 keV nm−1 is much more than that of nuclear energy
loss of 0.50 keV nm−1 , 0.61 keV nm−1 for bismuth and iron,
respectively.
In this paper, we present the first experimental evidence of
initial surface smoothing, thereafter roughening and sputtering
of immiscible Fe/Bi bilayer system by SHI irradiation. It is
also shown that the observed broadening of the Bi peak in RBS
spectra is due to the surface roughening at higher fluences.
2. Experimental details
We deposited a 58 nm Fe film on the Si (1 0 0) substrate
using the electron beam evaporation technique. Then 40 nm
of Bi film was deposited on Fe by the resistive heating
method without breaking the vacuum. Prior to deposition,
the Si sample pieces were properly cleaned and chemically
etched. The film thickness is evaluated during evaporation
2
A Gupta et al
by a calibrated quartz crystal thickness monitor. The films
were deposited in a high vacuum chamber at a base vacuum
of ∼10−6 Torr. The samples were irradiated by 120 MeV Au
ions at different fluences ranging from 3 × 1013 ions cm−2
to 1 × 1014 ions cm−2 at RT). The irradiation flux was kept
low (
1010 ions cm−2 s−1 ) to avoid sample heating during
irradiation. The electronic and the nuclear energy loss values
of the projectile were calculated using the Monte Carlo SRIM-
2006 code [23]. The projected range of 120 MeV Au ions is
10.84 µm and 7.05 µm for Bi and Fe, respectively, and thus,
the ions would penetrate deep within the Si substrate. The
thickness and the composition of the pristine and irradiated
samples were analysed by means of Rutherford backscattering
spectrometry (RBS) using 1.35 MeV He+ ions. The energy
spectrum of the backscattered He+ ion was measured using a
silicon surface barrier detector under an angle of 160◦ with
respect to the normally incident ion beam. The concentration
profiles were extracted from the RBS spectra with the help
of the ‘RUMP’ simulation code [24]. The concentration
profiles of Fe were fitted with a Gaussian error function and
the variances were determined. The observed increase in the
variance
σ 2 (ϕ) = σ 2 (ϕ) − σ 2 (0) was taken as a measure
for the mixing effect (where σ 2 (ϕ) and σ 2 (0) are the variances
of irradiated and pristine samples, respectively, and ϕ is the
fluence). Glancing angle x-ray diffraction (GAXRD) analysis
was performed using Cu Kα (wavelength λ = 0.154 18 nm)
radiation using Brucker D8 advance x-ray diffractometer to
study the mixed phase and crystallinity of film. GAXRD
measurements in the 2θ range of 20◦ –60◦ of as-deposited as
well as irradiated Fe/Bi films were performed at a grazing
angle of 2◦ with a scan speed of 0.5◦ min−1 and a step value of
0.02◦ . Atomic force microscopy (AFM) and scanning electron
microscopy (SEM) with x-ray dispersive energy analyzer
(EDAX) measurements were carried out to study the surface
morphology of the samples at IUAC, New Delhi and IIT
Roorkee, respectively.
3. Results and discussions
3.1. Glancing angle x-ray diffraction
The x-ray diffraction (XRD) pattern for the as-deposited
sample shows the emergence of two peaks at 27.17◦ and 44.76◦ ,
which are indexed as the (0 1 2) plane of the rhombohedral
phase of Bi and the (1 1 0) plane of the body centred cubic
(BCC) phase of Fe, respectively. It is observed from the XRD
spectra that the signal from Fe layers was always very weak
relative to that from Bi, because the atomic number of Bi is
large, so the atomic scattering factor of Bi is much higher than
that of Fe [25]. The intensity of the XRD peak of Bi improves
at a lower fluence up to 3 × 1013 ions cm−2 due to the increase
in crystallinity. However, the intensity decreases with a further
increase in fluence beyond 3 × 1013 ions cm−2 , which can be
attributed to the strain induced by energy deposition by SHI,
which results in a decrease in crystallinity of Bi. The average
size of the particles is estimated using Scherrer’s formula [26]
given by
kλ
D= , (1)
β cos θB
J. Phys. D: Appl. Phys. 41 (2008) 215306 A Gupta et al

Table 1. Average particle size of Bi and Fe estimated by Scherrer’s 3.2. Rutherford backscattering spectrometry
formula.
A typical RBS spectrum of Fe/Bi bilayer samples before and
Fluence FWHM Grain size FWHM Grain size
(ions cm−2 ) of Bi of Bi (nm) of Fe of Fe (nm) after irradiation by 120 MeV Au ions at different fluences is
shown in figure 2. Variance and interface broadening first
Pristine 0.3532 26.7 0.7800 11.3 decreases and then increases with ion fluences as shown in
3 × 1013 0.3265 30.1 0.7718 11.4
the inset of figure 2. A detailed analysis showed that the
6 × 1013 0.3336 29.2 0.6241 14.3
1 × 1014 0.3351 29.0 0.4982 18.5 Bi peak in the pristine sample could not be fitted accurately
because of a large tail, which could be attributed either to the
interface roughness or to the asymmetric granular nature of
the Bi film. In fact, while Fe evaporation onto Si results in a
smooth layer [28], Bi shows an island growth when evaporated
onto Fe and thus forms a rough surface. RBS spectra of the
pristine sample exhibited a long tail at the low energy edge
of the Bi peak, which indicates an extreme roughness with a
non-Gaussian height distribution. RBS analysis revealed that
steepness of the low energy edge of the Bi signal increases
at the fluence of 3 × 1013 ions cm−2 and beyond this fluence
the slope of the rear edge decreases with fluence. As can be
seen in figure 3, the tail area (integrated counts from zero to
50% of the low energy edge of Bi) also decreases initially for
the irradiation fluence of 3 × 1013 ions cm−2 and thereafter it
increases with increasing fluences. The increased steepness is
due to smoothing induced at low fluence, however, the decrease
in slope of the rear edge beyond 3 × 1013 ions cm−2 fluence
shows an increase in surface roughening.
Figure 1. GAXRD patterns of as-deposited and irradiated Fe/Bi As observed in many other ion mixing experiments, the
films on the Si (1 0 0) substrate. 2
edges at the interface are less steep after irradiation, i.e. σRBS
increases with increasing ion fluence. However, one should
where k is the Scherrer factor (0.9), λ = 1.5418 Å (for Cu 2
note that σRBS is composed (σRBS2
= σd2 + σmix
2
) of the variance
2
Kα ), β = FWHM (in radians) and 2θB is the Bragg angle. of the interfacial concentration gradient, σmix , and the lateral
The FWHM and particle size corresponding to the (0 1 2) and fluctuation of the top layer thickness, σd2 , which itself contains
the (1 1 0) XRD peaks in all cases are given in table 1. The both the interface and the surface roughness [29]. Therefore,
GAXRD spectra of irradiated films, as shown in figure 1(b), in the present case, the broadening at higher fluences may be
reveal a decrease in the FWHM (shown in table 1) with a lower the result of interface mixing, surface roughening and/or the
fluence. The average particle size of both Bi and Fe in this case effect of both. As observed, the large tail in the RBS spectra of
is estimated using equation (1) and the growth of Bi from 26.7 the pristine film may be due to the island structure and surface
to 30.1 nm is observed at the ion fluence of 3 × 1013 ions cm−2 . roughness in the Bi layer. To confirm this we characterized our
The spectra of irradiated films, as shown in figures 1(c) and (d), samples by AFM and SEM. We have also extracted the value
show an increase in FWHM (shown in table 1) with a higher of surface roughness using AFM and investigated the effect of
ion fluence from 6 × 1013 to 1 × 1014 ions cm−2 . The average surface roughening on interface broadening in RBS spectra.
particle size of Bi in these cases is estimated to be 29.2 nm and
29.0 nm, respectively. 3.3. Atomic force microscopy
SHI irradiation on the Fe/Bi system causes electronic The surface morphology of the as-deposited and irradiated
energy loss due to inelastic collisions of high energy ions films is shown in figure 4. The topography of the as-deposited
with the host atoms and introduces either point defect, defect film shows very high (up to 200 nm) structures at the surface
clusters or induces strain energy depending on the amount and has a large value of surface roughness of 23.6 nm.
of energy deposited [27]. In other words, when a SHI Bismuth grains of various sizes are present in the as-deposited
penetrates a solid, the material along the ion trajectory of film. These particles result in a non-Gaussian surface height
the ion beam is modified, atoms are pushed out of their distribution and are responsible for the long tail of the
normal positions and ordered structures such as that of the RBS signal (as discussed above). At the lower fluence
crystal lattice may be destroyed. It has been shown that the of 3 × 1013 ions cm−2 , there is an apparent decrease in the
material properties get altered due to the energy deposition root mean square (rms) roughness from 23.6 to 16.9 nm,
by the ion beam. The decrease in particle size in the Fe/Bi which may be attributed to ion induced smoothing of the
system with SHI irradiation at higher fluences from 6 × 1013 to surface. However, with a further increase in the fluence up
1×1014 ions cm−2 clearly indicates distortion in lattice caused to 1 × 1014 ions cm−2 , a significant increase in the surface
by stress-induced defects due to the increase in total energy roughness (from 16.9 to 32.1 nm) is observed. The variation
deposition (Se × ϕ) by the ion beam. of roughness versus ion fluence is shown in figure 5.

3
J. Phys. D: Appl. Phys. 41 (2008) 215306
Figure 2. RBS spectra of Fe/Bi film on the Si (1 0 0) substrate after being irradiated with 120 MeV Au ions of different fluences at RT and
the inset shows the variance σ 2 of the depth profiles and interface broadening
σ 2 extracted from the RBS data versus the fluence.
Figure 3. Area of tail of the Bi edge in the RBS spectra versus the
ion fluence for Fe/Bi on the Si substrate irradiated by 120 MeV Au
ions.
3.4. Scanning electron microscopy
SEM images of the as-deposited and irradiated Fe/Bi samples
on the Si substrate are shown in figures 6(a) and (b) and
corresponding EDAX profiles are also shown in figures 6(c)
and (d), respectively. The SEM image of pristine film shows
the formation of a continuous porous film. Micrographs of
pristine and irradiated samples clearly demonstrate that there
is a decrease in the surface roughness after gold ion irradiation.
4
A Gupta et al
This result supports the AFM analysis, which also shows the
decrease in the surface roughness at lower fluences.
The results obtained in this work from RBS and AFM
analyses of Fe/Bi bilayers strongly support this interpretation.
As mentioned above, the broadening obtained from RBS
2
measurements,
σRBS , may contain two contributions:
interface mixing and surface roughening. In most analyses
of IBM experiments, it has been implicitly assumed that
surface roughening and recrystallization of the top layer by
the impinging ion beam is unimportant as compared with
the strong interface mixing effect. However, in systems
where a small or even vanishing mixing effect is expected,
a quantitative separation of the two effects is necessary as
was shown by Sun et al [30]. They investigated IBM in
nitride/Al and Al/nitride systems and found that about 50%
of the broadening observed in the RBS spectra was due to
irradiation induced surface roughening. Upon comparing
2 2
the quantities
σRBS and
σAFM obtained for Au-irradiated
Fe/Bi bilayers, it also turns out that the broadening observed
with RBS is to a large extent determined by an increasing
surface roughness. The difference in
σRBS 2
−
σAFM
2
can be
regarded as a direct measure of the interface mixing or surface
roughening effect and is plotted in figure 7 (versus fluence).
It is clear from figure 7 that interface broadening in the RBS
spectra is due to the surface roughening induced by SHI.
We have also calculated the sputtering yield of Bi from
the change in the film thickness upon irradiation (measured
by RBS in terms of areal density (at cm−2 )). The sputtering
yield of Bi is found to be ∼200 at ion−1 at a lower fluence and
∼94 at ion−1 at the highest fluence (1 × 1014 ions cm−2 ). This
may be the reason for the low energy edge of Fe in RBS spectra
J. Phys. D: Appl. Phys. 41 (2008) 215306
Figure 4. (a) AFM image of the Fe/Bi sample unirradiated, (b) irradiated at 3 × 1013 ions cm−2 , (c) irradiated at 6 × 1013 ions cm−2 and
(d) irradiated at 1 × 1014 ions cm−2 , respectively.
Figure 5. Roughness versus fluence graph of Bi films as-deposited
and irradiated by 120 MeV Au ions.
being shifted towards high energy. However, smoothing of the
top layer narrows down the broadening of the Fe peak. The
combined effect results in shifting in the rear edge of Fe to
high energy without any visible overall shift of the Fe peak for
3 × 1013 ions cm−2 fluence.
5
A Gupta et al
According to the thermal spike model, a cylindrical molten
region is formed within the vicinity of the ion trajectory in
both the layers because both Fe and Bi are Se sensitive. This
is evident from figures 8 and 9, which show results obtained
from the thermal spike calculations for individual layers. We
extract the track diameter of 10 nm for Bi and 2 nm for Fe
for a few picoseconds from these figures. Although thermal
spike calculation reveals the formation of transient molten
state, the mobile atoms in the excited regions contribute to
smoothing instead of mixing due to positive heat of mixing.
It was reported earlier that in a miscible system strong mixing
takes place because of the transient molten state. However, in
our case, the system has a positive heat of mixing and hence
we do not observe mixing even though both the layers are Se -
sensitive and go to the molten state (as seen in figures 8 and 9).
A similar observation was also reported by Paulus et al [31] (Bi
on Si and SiO2 ) and Nakatani et al [32] (Bi or Au/oxide) that
chemical driving forces suppress interdiffusion in the molten
ion track.
When SHI passes through material ions transfer their
energy to the electrons in 10−17 s and the electrons reach an
equilibrium state in a time of the order of 10−15 s. Finally the
energy is transferred to the atomic lattice by electron–phonon
coupling. Therefore, the excess heat gets generated by SHI
irradiation within this localized region. The local temperature
J. Phys. D: Appl. Phys. 41 (2008) 215306
Figure 6. (a) SEM image of the Fe/Bi sample unirradiated, (b) irradiated at 1 × 1013 ions cm−2 , (c) EDAX pattern of the Fe/Bi sample
unirradiated and (d) irradiated at 1 × 1013 ions cm−2 .
2
Figure 7. Variation of effective mixing (
σRBS =
σd2 +
σmix
2
) which prevent interdiffusion across the interface during the
versus ion fluence using 120 MeV Au ions.
of the system gets increased by an amount of
T and the
heat gets transferred to the lattice in the form of energy via
electron–phonon coupling. Considering small grain volumes
of the Fe–Bi system we suppose that the heat gets confined
within the grain volume [33]. This gives rise to a non-
equilibrium state [34], which as a consequence increases the
6
A Gupta et al
volumes of the grains resulting in grain agglomeration at
higher fluences. This spectacular increase in surface roughness
may also be attributed to the effect of ions arising from
the electronic excitation-induced shear motion of the atoms
towards the surface, which could result in agglomeration on
the surface. Our AFM results are also in good agreement with
this explanation.
4. Conclusions
We have investigated SHI irradiation effects: surface
smoothing and subsequent roughening and sputtering of the
immiscible Fe/Bi bilayer system. We did not observe any
mixing in this system, although Fe and Bi are both known
to be sensitive to high electronic energy deposition by SHI.
We conclude from RBS and AFM results that SHI irradiation
induced smoothing and subsequent roughening and sputtering.
This can be explained on the basis of positive heat of mixing
transient thermal spike.
Acknowledgments
A Gupta and R S Chauhan are highly grateful to Inter-
University Accelerator Centre, New Delhi, for providing the
financial support for this work under the UFUP project. The
authors would also like to thank M Toulemonde, CAEN,
J. Phys. D: Appl. Phys. 41 (2008) 215306
Figure 8. The evolution of lattice temperature with time in 120 MeV Au ion irradiated Fe as calculated by the thermal spike model. Tm is
the melting temperature of Fe.
Figure 9. The evolution of lattice temperature with time in
120 MeV Au ions irradiated Bi as calculated by the thermal spike
model. Tm is the melting temperature of Bi.
France, for allowing them to use the code of thermal spike
calculations, and R Chandra for providing the SEM facility.
D K Avasthi would like to give sincere thanks to the
Department of Science and Technology for providing the XRD
system at IUAC, New Delhi, under IRPHA project to boost
research activities.
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