Gate control of ferromagnetic insulating phase in lightly-doped La0.875Sr0.

125MnO3−δ
film
H. Kuang, J. Wang, F. X. Hu, Y. Y. Zhao, Y. Liu, R. R. Wu, J. R. Sun, and B. G. Shen

Citation: Applied Physics Letters 108, 082407 (2016); doi: 10.1063/1.4942803

View online: http://dx.doi.org/10.1063/1.4942803
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 APPLIED PHYSICS LETTERS 108, 082407 (2016)

Gate control of ferromagnetic insulating phase in lightly-doped

La0.875Sr0.125MnO32d film
H. Kuang, J. Wang,a) F. X. Hu,a) Y. Y. Zhao, Y. Liu, R. R. Wu, J. R. Sun, and B. G. Shen
Beijing National Laboratory for Condensed Matter Physics and State Key Laboratory of Magnetism,
Institute of Physics, Chinese Academy of Sciences, Beijing 100190, People’s Republic of China
(Received 2 November 2015; accepted 14 February 2016; published online 26 February 2016)
The electric field effect on the lightly doped La0.875Sr0.125MnO3d (LSMO) thin film in electric
double-layer transistors was investigated by measuring transport properties of the film under vari-
ous gate voltages. It was found that the positive gate bias leads to an increase of the charge-orbital
ordering (COO) transition temperature and a decrease of the Curie temperature TC, indicating the
suppression of ferromagnetic metal (FMM) phases and preference of COO/ferromagnetic insulator
(FMI) with the hole depletion by gate bias. Such different electric field effects can be ascribed to
the weakening of the ferromagnetic interaction and enhancement of Jahn-Teller (JT) distortion
caused by the transformation of JT inactive Mn4þ-ions to JT active Mn3þ-ions. Moreover, a step-
like increase in the high temperature region of the q-T curve, which is related to the transition of
cooperative JT distortion, was found to develop with increasing the positive bias, indicating that
the cooperative JT distorted phase is stabilized by the depletion of holes in LSMO film. These
results demonstrate that the modulation of holes via electric field strongly affects the balance
between energy gains of different interactions and thus produce different effects on the competing
FMI, FMM, and cooperative JT distorted phases in LSMO film. V C 2016 AIP Publishing LLC.

[http://dx.doi.org/10.1063/1.4942803]

Hole doped-La1xSrxMnO3 exhibits various phase tran- ordering plane required by the concurrent JT effect with the
sitions due to the strong coupling among charge, spin, or- formation of COO.9–11 More recently, Wang et al. achieved a
bital, and lattice. In the lightly doped zone, two successive COO transition in the (001)-oriented La0.875Sr0.125MnO3/
structural phase transitions occur from a high temperature PMN-PT thin film by introducing a large in-plane tensile
pseudocubic phase to an intermediate Jahn-Teller (JT) dis- strain and breaking out of the straitjacket from substrate.12
torted orthorhombic phase and then to a low temperature These experiments demonstrated that the epitaxial strain and
pseudocubic phase. The most striking feature in this type of resulted lattice distortion is a key factor that influence the FMI
materials is the observation of the charge orbital ordering phase and COO transition in La0.875Sr0.125MnO3d (LSMO)
and insulating property in a ferromagnetic background. thin films. However, introducing extra lattice strain from vari-
Specifically, when x ¼ 0.125, a phase transition from para- ous substrates might bring about additional parameters such
magnetic to ferromagnetic accompanying an insulator to as defects, microstructures, and so on, which restricts the fur-
metal transition occurs at around 183 K (Refs. 1–3) which is ther investigation on the mechanism underlying various inter-
well explained by the double-exchange (DE) mechanism. At esting properties in lightly doped La1xSrxMnO3 film.
a lower temperature of about 150 K, another metal to insula- On the other hand, the carrier density is a key parameter
tor transition occurs in the ferromagnetic region which that controls the physical properties of manganites.
results in a ferromagnetic insulating (FMI) phase in the low Experiments showed that the modulation of carrier concen-
temperature region.1–3 This FMI phase cannot be explained tration by carrier doping in manganites could result in vari-
solely within the framework of the DE mechanism. Many ex- ous interesting phenomena including the charge orbital
perimental and theoretical studies have revealed that charge ordering.13,14 Recently, lots of interest has been focused on
and orbital ordering (COO) takes place in this FMI phase, electrostatically modulating physical properties of manganite
accompanying with the localization of charge carriers and thin film by using the configuration of electric field transis-
strong distortion of MnO6 octahedra.2,4–6 Meanwhile, experi- tors.15–17 In particular, many attempts have been made in the
ments showed that the properties of La0.875Sr0.125MnO3 thin research of electric field effect using all oxide-based field
film vary greatly from that of the bulk materials due to the effect transistors (FETs), composed of manganites and
epitaxial strain from the mismatch between the substrate and dielectrics/ferroelectrics, either for control of the different
the thin film. Particularly, the COO-induced metal-insulator phases or for developing new electronic devices.18–22
(MI) transition is suppressed in the (001)-oriented films due Different from the conventional chemical doping which is
to the clamp of the in-plane lattice by the substrate7–9 but is most widely used to modulate the charge carrier concentra-
achieved in (011)-oriented film by introducing anisotropic tion, electric field approach does not introduce impurity and
strains which allows a lattice deformation within the orbital can continuously change the charge carrier concentration by
varying the gate voltage. However, the low available gate
a)
Authors to whom correspondence should be addressed. Electronic bias and the inherent Thomas-Fermi screening effect23 pre-
addresses: [email protected] and [email protected] vent its further application on the manganite thin film. More

0003-6951/2016/108(8)/082407/5/$30.00 108, 082407-1 C 2016 AIP Publishing LLC

V

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 082407-2 Kuang et al. Appl. Phys. Lett. 108, 082407 (2016)

recently, quite a number of experimental investigations dem- reason for such preference. These unexpected results indicate
onstrated that the electric double-layer transistor (EDLT) is a that the modulation of carriers (holes) strongly affect the sta-
good alternative to the FETs for controlling the properties of bility of the cooperative JT distorted phase in LSMO film.
the manganites via carrier density modulation.24–32 To form The thin LSMO film was deposited on a (001)-oriented
an EDLT device, the ionic liquid/electrolyte is used as the single-crystal substrates of SrTiO3 by the pulsed laser depo-
gate dielectric materials instead of the conventional solid sition (PLD) technique. A KrF excimer laser (k ¼ 248 nm)
dielectric. Compared with the traditional solid dielectric, with a pulse energy of 180 mJ and a frequency of 2 Hz was
ionic liquids or electrolytes can provide very high electric used to ablate the stoichiometric target. The LSMO target
fields and thus a large modulation of the carrier density (up to was prepared by conventional solid reaction method. During
1014–1015 cm2) before breakdown occurs,27,28 which consid- the deposition, the temperature of the substrate was kept at
erably enlarge the research range of carrier concentration. 700  C and the oxygen pressure at 0.01 Pa. After deposition,
Some investigations have been performed on FETs configura- the film was cooled down to room temperature in vacuum.
tions composed of ionic liquid and manganite films.26–28,30–32 Considering the tradeoff between a large electric field effect
However, most of previous researches focused on the gate and a small resistivity of the film, we used the film with
control of insulator-metal transition (accompanied with the 20 nm thickness to fabricate the device and performed trans-
establishment of ferromagnetic ordering) and related percola- port investigations. The crystalline structure of the film was
tive transport in specific systems. There has been no report so checked by means of X-ray diffraction (XRD) using Cu-Ka
far on using EDLT to explore the effect of carrier modulation radiation on Bruker AXS D8-Discover. Meanwhile, the sur-
(field effect) on the competing various phases and correspond- face morphology of the film was investigated by atomic
ing transport properties in the low-doped LSMO with strong force microscopy (Seiko-SPA400). Magnetization was meas-
coupling among charge, spin, orbital, and lattice. Moreover, it ured with a superconducting quantum interference device
has been previously demonstrated that the electrostatically (SQUID-VSM). The sample was patterned using photoli-
doped carriers are more localized than those induced by chem- thography into a standard Hall-bar geometry with the side
ical doping.30 Thus, to investigate the evolution of the trans- gate set next to the channel. The schematic of the sample is
port behavior of the lightly hole-doped LSMO film under the illustrated in Fig. 1(a). A droplet of ionic liquid, DEME-
EDLT configuration would be unique and quite helpful for TFSI, was used to cover both the channel and the gate ena-
understanding the complex competition and related mecha- bling the ions to move freely as a gate voltage was put on
nism among the specific COO(FMI), ferromagnetic metal (see Fig. 1(b)). When a positive gate voltage is applied, the
(FMM), and JT-distorted phases. ion migration in DEME-TFSI depletes holes in the LSMO
In this letter, we present a report of the electric-field-con- channel. In contrast, a negative voltage results in accumula-
trol of the competing FMI, FMM, and JT distorted phase in tion of the holes in the channel. The gate voltage dependent
the lightly doped LSMO thin film by modulating the carrier
concentration. A EDLT device with LSMO as channel was
used to investigate the transport properties under various gate
voltages. The N, N-diethyl-N-methyl-N-(2-methoxyethyl)am-
monium bis(trifluoromethylsulphonyl)imide (DEME-TFSI),
which is a binary salt with high polarity and composed of
nitrogen-containing cations and imide anions, was chosen as
the ionic liquid due to its higher dielectric constant and ionic
conductivity than other electrolyte dielectrics. Moreover, it is
solvent-free and can be used on lots of materials, especially
suitable for manganite oxide films, on which it can be exposed
to moderate voltages avoiding redox reactions. Our results
revealed that the hole depletion induced by positive gate bias
favors the FMI state and suppresses the FMM phase.
Moreover, we found that the highly insulating state induced
by positive gate voltage cannot return back to the original
state after the positive voltage was removed and a negative
one was even applied. Such interesting phenomena can be
ascribed to the different accumulation and migration effect of
oxygen vacancies driven by different polarities of the bias,
which results in an irreversible oxygen vacancy distribution
and thus an irreversible resistivity behavior in the channel film
of LSMO. Furthermore, an unusual step-like change in the
q-T curve, which is supposed to be related to the transition of
cooperative JT distortion, was found to develop with the posi-
tive gate bias applied. Further applying negative bias resulted
in the disappearance of such cooperative JT distortion transi-
tion. The induced transition between JT active Mn3þ and inac-
tive Mn4þ ions by carrier injection was regarded as the main FIG. 1. The schematic illustration of the (a) patterned sample and (b) EDLT.

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 082407-3 Kuang et al. Appl. Phys. Lett. 108, 082407 (2016)

after the gate voltage was kept for 30 min at 300 K to ensure
a sufficient migration of the polarized ions in DEME-TFSI.
During the measurements, the gate voltage was kept as the
sample was cooled down.
To suppress the influence from the lattice mismatch, we
chose the single crystalline SrTiO3 (STO) which has a very
small lattice mismatch with LSMO as the substrate for the
growth of LSMO film. Figure 2(a) shows an X-ray h-2h scan
profile of the 20 nm-thick LSMO film, which indicates that the
film was epitaxially grown on the substrate and no other
phases or textures are observed. The reflections from the film
were found to overlap with those from STO substrate com-
pletely, which indicates a nearly pseudomorphic growth and
small strain induced by substrate taking into account that lat-
tice parameters of LSMO (a ¼ 3.902, b ¼ 3.907, c ¼ 3.896) are
very close to that of the STO (a ¼ 3.905). The surface mor-
phology is investigated by atomic force microscopy (AFM).
The surface roughness RMS was found to be 0.9 nm, indi-
cating the good quality of the film. The resistance and magnet-
ization versus temperature curves for the film are shown in
Fig. 2(b). Two successive MI transitions were identified from
the R-T curve. The one in the higher temperature happens in
the vicinity of the Curie temperature, and another in the lower
temperature suggests a COO transition.2–4 The low oxygen
pressure during the deposition and post annealing leads to oxy-
gen deficiencies in the film, which increases the distortion of
MnO6 octahedra and reduces the influence from the substrate,
FIG. 2. (a) X-ray diffraction pattern of the LSMO/STO structures. (b) The promoting the formation of charge-orbital ordering at low tem-
original temperature-dependent resistance and magnetization curves of the perature. Previous researches have demonstrated that the COO
LSMO film. transition at low temperature could be induced by either epi-
taxial strain or deficiencies.12,33
transport properties were measured in the SQUID-VSM with Figure 3 presents the temperature-dependent resistance
in situ electric fields applied on the gate. The measurements (q-T) for different applied gate voltages measured on a
were carried out in the sequence of positive gate voltages, 20 nm thick LSMO channel. Firstly, one can find that the re-
zero, and negative ones. All measurements were performed sistance in the original state shows a bulk-like behavior

FIG. 3. Temperature dependent resis-

tivity for (a) the positive gate bias and
(b) the negative gate bias. (c) The
details of (a), showing the detail of the
abnormal change in resistivity related
to cooperative JT distortion. (d) The
gate voltage dependent TC and TCOO
upon positive bias.

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 082407-4 Kuang et al. Appl. Phys. Lett. 108, 082407 (2016)

similar to the one measured on the as-prepared film. Various electrochemical reaction between the ionic liquid and the
positive gate voltages were applied to the channel through channel film.
the gate electrode which is connected with the channel by Moreover, the successive metal-insulator transitions,
the ionic liquid. As shown in Fig. 3(a), the resistance of the related to the formation of ferromagnetic ordering and charge-
channel shows an increase in the whole measurement range orbital-ordering, respectively, show different responses to the
with the application of positive gate voltage, which should gate bias. It was found that the peak temperature for the transi-
be ascribed to the reduction in the carrier concentration tion at higher temperature region (Curie temperature TC,
due to the gate voltage induced depletion of holes in the defined as the maximum point where dq/dT ¼ 0) shifts towards
LSMO channel. Meanwhile, with the increase of the gate lower temperature (from 234 K to 188 K) when the gate volt-
voltage, the channel film gradually converts into a complete age increases from 0 V to þ3.0 V. On the contrary, the transi-
insulating state. Specially, when the gate voltage reaches tion point of the MI transition at low temperature (TCOO,
þ3 V, a highly insulating state appears in the entire tempera- defined as the minimum point where dq/dT ¼ 0) first decreases
ture range and an obvious plateau is observed in the q-T to a lower temperature of 132 K at the voltage of þ1.5 V and
curve. Since LSMO is hole-doped, when a positive gate volt- then shifts progressively to higher temperatures (from 132 K to
age is applied, holes in the channel are depleted (see Fig. 154 K, see Fig. 3(d)) with further increasing the gate voltage.
1(b)), resulting in the reduction of carrier concentration. Such opposite variations in TC and TCOO indicate that the posi-
Measurements of Hall effect were performed in the LSMO tive gate voltage can suppress the FMM state and favor the
Hall bar in order to estimate the sheet carrier concentration COO state via reducing the concentration of charge carriers.
ns. The ns values under zero gate voltage were calculated to Actually, the reduction of carrier (hole) concentration leads to
be in the range of 1.8  1014 to 7.2  1014 cm2 for different a weaker ferromagnetic interaction according to DE mecha-
temperatures, whose magnitudes are consistent with previous nism and thus the suppression of ferromagnetic ordering.13 As
reports for mixed-valence manganites.24,28 Furthermore, it a result, the FMM transition temperature decreases with the
was found that the calculated carrier density decreases by an increase of gate voltage. On the other hand, the depletion of
order of magnitude, while a positive gate voltage of þ2 V holes turns JT inactive Mn4þ-ions to JT active Mn3þ-ions,3
was applied on EDLT. Specially, the modulation of sheet which introduces JT distortion in the MnO6 octahedra around
carrier density upon þ2 V is as large as 6.4  1014 cm2 at the Jahn-Teller active site. Thus, with increasing the gate volt-
300 K. Such value of the modulated carrier density is at least age, the lattice distortion is largely enhanced, which causes the
ten times more than that can be achieved from conventional channel film to favor the COO state at low temperature and
gate dielectrics and surely will cause the increase of channel thus an increase of TCOO.12 The observed opposite shift of TC
resistance. Opposite effect is expected for the negative gate and TCOO with the increase of the negative gate voltage (see
voltage. As shown in Fig. 3(b), the resistance of the channel Fig. 3(b)) further supports such explanations.
decreases monotonously in the whole measuring temperature Interestingly, upon cooling, a step-like increase of the re-
range with the increase of the magnitude of the negative gate sistance appears around 298 K when a voltage of þ1.5 V is
voltage, which should be ascribed to the negative gate volt- applied on the gate electrode, indicating a discontinuous transi-
age induced injection of holes from the interface between tion. With further increase of the gate voltage, such discontinu-
ionic liquid and the channel film. However, the film remains ous transition keeps and its start-point moves slightly towards
the highly insulating state and cannot return back to the orig- low temperature (see Fig. 3(c)). However, when a negative
inal state even at a voltage of 2.5 V. Such different situa- voltage was applied on the gate electrode, such discontinuous
tion for positive and negative gate voltage might be related transition disappears. Previous researches by resonance X-ray
to the migration of the oxygen vacancies in the channel film. scattering on the bulk LSMO2,3,36 have confirmed that this
Positive (negative) gate bias polarity will drive the oxygen transition is related to the appearance of cooperative JT dis-
vacancies to migrate away from (towards) the interface, torted phase. However, such a transition was scarcely observed
hence resulting in different distribution of oxygen vacancy in LSMO thin films probably due to the limitation of coopera-
and lattice distortion. Considering the oxygen vacancies tive JT distortion by the substrate. In this study, applying posi-
could affect the doping intensity,34,35 such different distribu- tive gate voltages introduces much more distorted MnO6
tion would lead to different carrier mobility and thus differ- octahedra in the channel film via turning JT inactive Mn4þ-
ent conductivity in the channel. Moreover, previous research ions to active Mn3þ-ions by depleting holes as discussed
has demonstrated that the negative gate voltage can accumu- above, which will largely increase the energy gain connected
late oxygen vacancies at the interface,35 which will make the to electron-phonon interaction. As a result, the stability of the
distribution discrepancy caused by different bias polarity ir- cooperative Jahn-Teller distorted phase is enhanced and the
reversible to some extent. Thus, it might be reasonable that discontinuous phase transition appears around room tempera-
the resistance of the channel upon negative gate bias cannot ture. On the contrary, applying negative gate voltage induces
completely return back to the original one. Moreover, the hole doping in the LSMO thin film, turning Mn3þ-ions back to
compared atomic force microscopy investigations of the sur- Mn4þ-ions. As a result, the stability of the cooperative JT dis-
face quality of the channel film before and after the gating torted phase is reduced and the transition disappears in the
sequence show that no remarkable change occurs in the sur- measuring temperature range.
face morphology and the surface RMS roughness, which To conclude, we studied the electric field effect on the
suggests that the observed different transport behaviors competing phases in La0.875Sr0.125MnO3d thin film by
under positive and negative gate voltages should not be measuring transport properties of the EDLT device under
owing to the possible damage of the film induced by the various gate voltages. The results revealed that the depletion
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2016 05:03:01
 082407-5 Kuang et al. Appl. Phys. Lett. 108, 082407 (2016)

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