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Fermi level tuning and the robustness of topological surface states against
impurity doping in Sn doped Sb2Te2Se

Article in Applied Physics Letters · April 2021

DOI: 10.1063/5.0040697

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Fermi level tuning and the robustness of
topological surface states against impurity
doping in Sn doped
Cite as: Appl. Phys. Lett. 118, 154001 (2021); https://doi.org/10.1063/5.0040697
Submitted: 15 December 2020 . Accepted: 20 March 2021 . Published Online: 12 April 2021

Debarghya Mallick, Shoubhik Mandal, R. Ganesan, and P. S. Anil Kumar

Appl. Phys. Lett. 118, 154001 (2021); https://doi.org/10.1063/5.0040697 118, 154001

© 2021 Author(s).
 Applied Physics Letters ARTICLE scitation.org/journal/apl

Fermi level tuning and the robustness

of topological surface states against
impurity doping in Sn doped Sb2Te2Se
Cite as: Appl. Phys. Lett. 118, 154001 (2021); doi: 10.1063/5.0040697
Submitted: 15 December 2020 . Accepted: 20 March 2021 .
Published Online: 12 April 2021

Debarghya Mallick, Shoubhik Mandal, R. Ganesan, and P. S. Anil Kumara)

AFFILIATIONS
Department of Physics, Indian Institute of Science, Bangalore 560012, India

a)
Author to whom correspondence should be addressed: anil@iisc.ac.in

ABSTRACT
In this work, we have studied the transport properties of two different single crystals, Sb2 Te2 Se and Sn-doped Sb2 Te2 Se. By analyzing the
Shubnikov–de Haas oscillations for the devices made from both the crystals, we have extracted the Berry phase. The non-trivial value of
the Berry phase for both the samples unambiguously indicates the robustness of the topological surface states against the impurity doping.
The parent compound is n-type due to excess Te vacancies, and we could show from the sign of the intercept in the Landau level fan diagram
and from the Hall effect measurements that doping with Sn makes it p-type. This demonstrates the tuning of the Fermi level in a topological
insulator upon Sn doping.
Published under license by AIP Publishing. https://doi.org/10.1063/5.0040697

Topological insulators are a new class of materials, which have
brought a new arena in the scientific community over the last decade
for their exotic properties and applicability in the field of quantum
computing and dissipationless electronics.1,2 Experimentally, from
Angle Resolved Photoemission Spectroscopy (ARPES) studies, the
gapless surface states and the gapped bulk states can easily be verified.3
The magnetotransport study with the Shubnikov–de Hass Oscillation,
which is the consequence of Landau Level (LL) formation, is another
probe to detect the topological surface states (TSSs) via the extraction
of the Berry phase.4 Thus, measuring the Berry phase will be a litmus
test to probe the linear band touching or the TSS in topological mate-
rial.4,5 Now, to unleash the full potential of TI, it has to work in the
ambient conditions where the unintentional impurity doping of the TI
surface is inevitable.6 Hence, it is very essential to check the robustness
of the topological surface states (TSSs) upon impurity doping.
Previously, the effect of ambiance on the TSS has been studied theoret-
ically and experimentally mostly by means of ARPES. It was estab-
lished that the topological order almost remains intact when the
sample is exposed to the ambient impurities.7,8
Bi2x Sbx Te3y Sey ðBSTSÞ has attracted a great deal of attention
in the last several years for having less bulk contribution to the con-
duction, making the Fermi level close to the Dirac point.9,10 But
another ternary compound, Sb2 Te2 Se, which was predicted to host an
odd number of Dirac cone on its surface, has received comparatively
much less attention.11 The ARPES study on this compound has
revealed that the TSS8 and magnetotransport study has shown
Shubnikov–de Haas (SdH) oscillation, from which the non-trivial
Berry phase was extracted to further confirm its topological nature.12
In this work, we have studied the magnetotransport of Sb2 Te2 Se
and then 1% Sn doped Sb2 Te2 Se, that is, Sb1:99 Sn0:01 Te2 Se. SdH oscil-
lations were observed for both the systems. It is well known that tin
doping creates an impurity band, which, in turn, increases the scatter-
ing at a large scale.16–18 Thus, our motive was to introduce Sn to
increase the scattering and to study the TSS by electrical means.
Despite doping with Sn impurities, it turns out that the Berry phase
retains the value p for the tin-doped sample as well, like the parent
crystal. This unambiguously signifies the robustness of the TSS of a TI.
Also, we showed that although Sb2 Te2 Se is p-type material in gen-
eral,12 since our material is having excess tellurium vacancies, it has
turned into an n-type material. However, Sn doping tunes the Fermi
level, making the system p-type again. This behavior gets reflected not
only in Hall measurements but also in the sign of the intercept in the
Landau Level fan diagram.19 Thus, these indicate that the Fermi level
tuning can be accomplished by Sn doping.
High-quality single crystals of Sb1:99 Sn0:01 Te2 Se and Sb2 Te2 Se
were grown by the modified Bridgman method. The procedure in
detail can be found elsewhere.12 The resultant shinny crystal was
cleaved easily along the c axis. X-ray diffraction (XRD) was performed

Appl. Phys. Lett. 118, 154001 (2021); doi: 10.1063/5.0040697 118, 154001-1
Published under license by AIP Publishing
 Applied Physics Letters
to ensure the phase and the orientation of the single crystal.
Stoichiometry was determined with the help of a JEOL Electron
Probe Micro Analyzer (EPMA) system. Then, mechanical exfolia-
tion was done using the scotch tape technique on an SiO2 (285 nm
thick)/Si(100) substrate. In order to make the device, we chose flat,
thinner, and bigger size crystals using an optical microscope. Then,
Hall bar designs were patterned using the standard electron beam
lithography technique. Cr/Au (10 nm/200 nm) contacts were given
using an electron beam evaporator system, and the samples were
mounted in an oxford 2 K cryostat for the magnetotransport
measurements.
The x-ray diffraction study confirms the single crystalline phase
(Fig. S1). From the Atomic Force Microscopy (AFM) study, the thick-
ness of the device is confirmed to be around 50 nm as shown in Fig.
1(a), which also shows the schematics of the longitudinal voltage and
the Hall voltage geometry along with the current probes. An Electron
Probe Micro Analyzer (EPMA) was employed to record the doping
percentage of Sn, which yields 1% Sn replacing Sb in Sb2 Te2 Se. The
longitudinal resistance (magnetoresistance) (Rxx) started increasing
classically with the increase in the magnetic field, showing no sign of
Weak Antilocalization (WAL) at the lower magnetic field [Fig. 1(b)].
This is consistent with the earlier reports of the parent compound.12,20
Now, to look into further why the TI material is not showing WAL,
we have to calculate how much the Dirac carriers (the surface states)
contribute to the total conduction. That is, we have to calculate the
ratio
surface conduction e:nSdh :lSdh
¼ ;
total conduction rxx :t
FIG. 1. Sn-doped Sb2 Te2 Se: (a) AFM image of the device. The longitudinal (Vxx)
and transverse (Hall,Vxy) geometries are also shown. (b)The perpendicular and par-
allel MR of the same sample. The parallel MR hardly shows any oscillation,
whereas the perpendicular MR has clear SdH oscillations. (c) SdH oscillations in
the reciprocal magnetic field at different temperatures. (d) Temperature dependence
of the SdH oscillation amplitudes at a particular magnetic field. Fitting with tempera-
ture dependence part of the Liftshitz-Kosevich formula yields the effective mass of
the electron. The inset shows the fast Fourier Transform corresponding to the oscil-
lation at 2 K.
Appl. Phys. Lett. 118, 154001 (2021); doi: 10.1063/5.0040697
Published under license by AIP Publishing
ARTICLE scitation.org/journal/apl
qxx
where rxx ¼ q 2 þq 2 and t is the thickness.20 This ratio yields 0.7%,
xx yy
which proves that the surface state contribution to the total conduc-
tion is very less; nevertheless, we will show later that the SdH oscilla-
tions stem from the surface states, not from the bulk. Moreover, we
can figure out the reason for the absence of WAL by finding the ratio
of the amplitude of the SdH oscillation (DrSdh ) to the total mean value
of the magnetoconductivity (rmean). The calculation yields
DrSdh
¼ 0:3%:
rmean jBmax
Hence, from both the ratios shown above, it is obvious that the total
conduction is dominated by the bulk carriers, not the surface carriers
(the Dirac carriers) since the Fermi level is away from the Dirac point
(In the Landau level fan diagram section, we will show that the
Landau level indices are pretty large), and therefore, very high bulk
domination in the conduction suppresses the WAL leaving the classi-
cal parabolic MR.20 The metallic nature of the Resistance vs tempera-
ture curve also indicates the dominating bulk conduction (Fig. S3). To
check whether the SdH oscillations stem from the TSS, we measured
the sample resistance with the magnetic field applied parallel to the
sample plane. Figure 1(b) shows the superposition of the perpendicu-
lar and the parallel MR data. It is evident from the figure that the oscil-
lation is hardly present in the parallel MR data. This unambiguously
indicates that SdH oscillations mainly arise from the TSS. The longitu-
dinal resistance ðRxx Þ has been converted into longitudinal conductiv-
ity ðrxx Þ with the help of a conductivity tensor
qxx
rxx ¼ (1)
qxx 2
þ qyy 2
(see Fig. S2). The reason, we dealt with the conductivity instead of
resistivity, is that the result might have been misleading if we take
resistivity while analyzing the LL fan diagram (LL fan diagram will be
discussed next) depending on the absolute value of rxx and rxy.22
Figure 1(c) shows the SdH oscillations after subtracting the back-
ground from the magnetoconductivity curve, and the conductivity
oscillates periodically with 1/B. It is evident that the amplitude is get-
ting reduced with an increase in temperature. Now, to fit the SdH
oscillations and the temperature dependence of its amplitude, we have
used the Lifshitz-Kosevich (LK) equation21,22 as follows:
 
k F 1
rxx / exp ðkD Þ cos 2p þ þcd
sinhk B 2
2p2 KB Tm (2)
where k ¼ ;
heB
2p2 KB TD m
kD ¼ :
heB
Here, F is the frequency of the oscillations after carrying out fast
Fourier transform (FFT) plotted in the reciprocal magnetic field (1/B)
[inset of Fig. 1(d)]. 2pc is the Berry phase, and d is the dimensional
parameter. d takes the value of 61/8 for 3D, and for 2D, it is zero.21
As we have discussed earlier, our material has 2D topological surface
states, which will allow us to take the value of d ¼ 0, and here, TD is
the Dingle temperature. In the LK equation, the first two terms are
there to take care of the damping part of the oscillation, whereas the
last part (the cosine function) takes care of the oscillatory nature and
118, 154001-2
 Applied Physics Letters
the phase associated with the oscillations. From the temperature
dependence of the amplitude of the oscillation, we can calculate the
effective mass or the cyclotron mass of the Dirac electron. Thus, we fit
the temperature dependence of the amplitude of the oscillation at a
fixed magnetic field (7.315 T) with rxx / k=sinhk, which yields the
effective mass as m ¼ 0.11 6 0.03 me, where me is the rest mass of the
electron [Fig. 1(d)]. Thus, it is evident that the electron acts like a
Dirac fermion in our material. The magnetic field dependence will
yield the Dingle time and LL broadening.23 We fit the magnetic field
dependence curve of the oscillation amplitude at a fixed temperature
(2 K) with rxx / expðkD Þ and extract the Dingle temperature (TD) to
be around 14 K and the Dingle time (sD) to be 9  1014 s [Fig. 2(a)].
These values are consistent with the previous reports in TI mate-
rial.20,23,24 The Dingle time basically is the relaxation time, that is, the
mean time interval between two successive collisions of the carriers
and LL broadening can be calculated from the Dingle temperature as
C ¼ pkB TD ¼ 4:76 meV.25 The linear Hall data [Fig. 2(b)] indicates
the single type of carrier, and the positive slope shows that the carrier
is hole. We have calculated the mobility (lHall) and the carrier concen-
tration (nHall) to be 4400 cm2 =V s and 3  1019 =cm3 from the Hall
data. However, the SdH mobility(lSdH) and SdH carrier concentration
(nSdH) are estimated to be 1500 6 45 cm2 =V s and 31014 =cm2 ,
respectively. Thus, the SdH mobility is almost three times less than the
same derived from the Hall effect. The reason is that the SdH mobility
takes care of the scattering at all the angles, whereas scatterings only at
large angles are considered in the Hall effect, which is only the large
energy transfer scattering that contributes to the Hall mobility, thereby
making the Hall mobility greater than the SdH mobility.4 Now, from
the oscillatory part of the Lifshitz–Kosevich formula [Eq. (2)], that is,
the cosine part, we extract the Berry phase to understand if the elec-
tron acts as a Dirac fermion. Here, 2pc is the Berry phase. We
extracted the Berry phase in two ways to check the self-consistency.
First, we fitted the SdH oscillations with the LK formula extracting the
FIG. 2. Sn-doped Sb2 Te2 Se: (a) Dingle plot with linear fitting, which yields the
Dingle time and the Dingle temperature. (b) Linear Hall effect indicating holes as
the carrier. (c) Liftshitz–Kosevich fit to the SdH oscillation at 2 K. The fit yields the
Berry phase and the Dingle temperature. LL indices are shown. (d) Landau level
fan diagram indicating the Berry phase.
Appl. Phys. Lett. 118, 154001 (2021); doi: 10.1063/5.0040697
Published under license by AIP Publishing
ARTICLE scitation.org/journal/apl
Dingle temperature to be 17 K, which is close to the value obtained
from the magnetic field dependence plot (14 K) and the Berry phase
(2pc) to be 0.41  2p ¼ 0.81p [Fig. 2(c)]. Second, we plotted the
Landau Fan diagram, which is the LL index vs the inverse of the mag-
netic field (1/B) plot [Fig. 2(d)]. Here, while indexing the Landau lev-
els, we followed the convention of assigning the integer value to the
minima of the oscillations.12 The intercept of the extrapolated straight
line to the LL index axis (y-axis) is of prime interest since this mani-
fests the Berry phase. It is clear from the inset of Fig. 2(d) that in our
case, the intercept is 0.4, which is close to the value derived from the
LK fitting of the SdH oscillation. The Berry phase, generally for non-
Dirac material, takes the value zero, but if the band structure of the
material contains the Dirac cone, then the Berry phase should be
p.13–15,28 So the value of the Berry phase can demonstrate the existence
of the Dirac cone or the topological nature of the electron in a topolog-
ical insulator. Thus, the nontrivial value of the Berry phase for our
case (0.8 6 0.1 p) proves the existence of topological surface states in
our material, Sb1:99 Sn0:01 Te2 Se. We can extract the Fermi wave vector
using the Onsager relation, F ¼ 2eh Kf2 , where F is the FFT value and Kf
1
is the Fermi vector. The Kf value is estimated to be 0.067 8 Å . We
also extracted Fermi velocity (vf) and mean free path (le) from the SdH
oscillations to be 7:15  105 m/s and 67 nm, respectively, using the
relations vf ¼ mh Kf and le ¼ vf sD .20,24 The Fermi energy can be cal-
culated for the Sn-doped material by using Ef ¼ m vf2 ¼ þ0:31 eV
(“þ” denotes the Fermi level in the conduction band).26,27 There are
oscillations in Hall data also, at the higher field. Analysis of that can be
found in the supplementary material (Fig. S3).
The control sample, that is, the undoped Sb2 Te2 Se single crystal,
was prepared using the same temperature profile as the other crystal,
and the exfoliated nanoflakes from the control sample were also mea-
sured in the same manner. SdH oscillations were obtained for different
temperatures and are presented in Fig. 3(a). The effective mass is
FIG. 3. The undoped sample (Sb2 Te2 Se): SdH oscillation analysis for the undoped
sample: (a) SdH oscillations in the reciprocal magnetic field at different tempera-
tures. (b) Temperature dependence of the oscillations amplitude. The inset shows
the FFT graph. (c) Dingle plot.
118, 154001-3
 Applied Physics Letters
derived to be m ¼ 0:1260:05me , me is the electron rest mass, from
the temperature dependence plot of the oscillation amplitude [Fig.
3(b)], and the magnetic field dependence of the oscillation amplitude
at the lowest temperature (2 K) yields the Dingle time of 8:8  1014
sec and the Dingle temperature of 14 K [Fig. 3(c)]. In the same
manner like the doped sample, the Fermi level can be estimated as
Ef ¼ m vf2 ¼ 0:34 eV (“” denotes the Fermi level in the valence
band).
The fast Fourier transform for the oscillations at 2 K is presented
in the inset of Fig. 3(b). The LK fit to the SdH oscillation at the lowest
temperature (2 K) yields the Berry phase of 0.55  2p ¼ 1.1p
[Fig. 4(a)]. The intercept of 0.51 in the Landau fan diagram yields the
Berry phase of 0.51  2p ¼ 1.02 (6 0.1)p, and the slope of the straight
line is also close to the FFT value as expected [Fig. 4(b)]. Now, the
striking difference between the undoped sample and the Sn doped
sample is the sign of the intercept in the Landau level fan diagram. For
the control sample, it is negative [inset of Fig. 4(b)], whereas in the
case of the doped one, it is positive [inset of Fig. 2(d)]. The sign of the
intercept in the LL fan diagram has been shown to carry the informa-
tion of the type of carrier present in the system.19 Hence, the negative
intercept for the control sample is indicative of electrons as the carrier.
This is corroborated by the Hall measurement as well [Fig. 4(c)].
Sb2 Te2 Se is derived from the parent material Sb2 Te3 by partially
replacing Te with Se, and both the compounds are generally reported
to be p-type.12 Here, in our case, the control sample has tellurium
deficiency (Sb2 Te1:9 Se1:1 ), which makes the system n-type. Moreover,
Sn-doping pushes the Fermi level to the valence band, making the tin-
doped sample a p-type material [Fig. 4(d)], and has already been
shown in the last section [Fig. 2(b)]. The carrier concentration and
mobility from the linear Hall effect are found to be 3  1019 =cm3 and
2264 cm2 =V s. The SdH mobility is comparatively less as expected,
1288 6 77 cm2 =V s.
In summary, we have performed the magnetotransport study on
nanoflakes exfoliated from two different single crystals, Sb2 Te2 Se and
1% Sn-doped Sb2 Te2 Se. SdH oscillations are observed on both the
FIG. 4. The undoped sample (Sb2 Te2 Se): (a) Lifshitz–Kosevich fit to the SdH oscil-
lation at 2 K. (b) Landau fan diagram. (c) Linear Hall data indicating electrons as
the carrier. (d) Schematics for Fermi level tuning by Sn doping.
Appl. Phys. Lett. 118, 154001 (2021); doi: 10.1063/5.0040697
Published under license by AIP Publishing
ARTICLE scitation.org/journal/apl
samples. Analysis of the quantum oscillations yields the non-trivial
Berry phase in both cases, establishing the fact that topological surface
states are robust against impurities. We also showed from the Landau
level fan diagram and from the Hall measurements that tin doping can
be efficiently utilized to tune the Fermi level. Thus, at a proper doping
concentration of Sn, without perturbing the topological surface states,
the Fermi level can be tuned to hit the Dirac point, and thereby, it can
be employed for the development of topological insulator-based spin-
tronic devices.
See the supplementary material for x-ray diffraction data of the
crystal, crystal image, magnetoresistance and magneto-conductivity
data with oscillations, and the analysis of Hall resistance oscillation.
D.M. and S.M. thank MHRD, Government of India. P.S.A.K.
acknowledges Nanomission, DST, India, for financial support. The
authors thank NNFC and MNCF, Centre for Nano Science and
Engineering and Advanced Facility for Microscopy and
Microanalysis (AFMM) at the Indian Institute of Science,
Bangalore, for fabrication and characterization.
DATA AVAILABILITY
The data that support the findings of this study are available
from the corresponding author upon reasonable request.
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