Results in Physics 13 (2019) 102228

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Results in Physics
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A study on optical properties of Sb2Se3 thin films and resistive switching T

behavior in Ag/Sb2Se3/W heterojunctions
Chunmin Liua, Yafei Yuana,b, Ling Chenga, Jing Sua, Xingtong Zhanga, Xiangxiang Lia,
⁎
Hao Zhanga,c, Min Xua,c, Jing Lia,c,
a
Department of Optical Science and Engineering, Fudan University, Shanghai 200433, China
b
Department of Electronic Engineering, Center for Intelligent Medical Electronics, Fudan University, Shanghai 200433, China
c
Shanghai Ultra-Precision Optical Manufacturing Engineering Center, Shanghai 200433, China

A R T I C LE I N FO A B S T R A C T

Keywords: In this study, optical phase change property and bipolar memristive switching behavior were systematically
Sb2Se3 thin films characterized in Sb2Se3 thin films with different annealing temperatures and Ag/Sb2Se3/W heterojunction, re-
Different annealing temperatures spectively. The structural investigations reveal that the crystallinity of Sb2Se3 sample improves with increasing
Optical properties annealing temperature. Anomalous changes of both structure and optical properties are attributed to the in-
Memristive switching behavior
crease of defect states at an excessively high annealing temperature. Additionally, the absorption edge shift
towards longer wavelength after thermal treatment, indicating a decrease in the optical band gap. In the aspect
of electrical characteristics, the Ag/Sb2Se3/W cell has a bipolar memristive switching behavior and shows re-
versible switching property. The study based on the optical properties and memristive switching behaviors of
Sb2Se3 thin films offers an important understanding to the applications of Sb2Se3 and other chalcogenide
semiconductor as promising materials for integrated optical system and chalcogenide-based memory devices.

Introduction including programmable analog circuits [15] and artificial neural

computing [16]. In the aspect of material selection, the function layer is
Chalcogenide thin films have drawn considerable attention in the critical to the characteristics of resistive switching (RS). As the most
past decades owing to their extensive applications in optical and elec- investigated materials, metal oxide series have been studied widely
trical devices such as phase change random-access memory, nonvolatile since the first memristor was demonstrated; however, the development
electronic memory, thin-film solar cells and super-resolution imaging trend of high-density storage requires the memory system to drive
[1–4]. However, as an element of the VI group, Se has disadvantages of scalable functions [2,17]. Therefore, chalcogenide-based RRAM devices
low sensitivity and short lifetime, which limits the applications of were put forward and showed important applications in Programmable
chalcogenide materials containing Se element to some extent. For- Metallization Cell. In the recent studies of our group, excellent resistive
tunately, it can be overcome by combining Se with elements into switching behaviors were successfully exploited in many chalcogenide-
compounds such as Sb, As and Ge [5]. Among them, Sb2Se3 is a layer- based RRAM devices, such as Sb2Te3-RRAM, In2Se3-RRAM, In2Te5-
structured semiconductor with orthorhombic phase, in which each Sb RRAM and so on [2,18,19]. For Sb2Se3, as mentioned earlier, most of
atom and each Se atom is surround by three opposing atoms [6–8]. the related studies are focused on the optical and phase change prop-
Several research groups have attempted to investigate the potential erties. Despite an attempt had been made to elucidate the memory
applications of Sb2Se3 in PCRAM [9], thermoelectric devices [10], switching behavior in Sb2Se3 thin films, the underlying memristive
photodetectors [11], photovoltaics [12] due to its excellent optical and mechanism of the Sb2Se3-RRAM has not yet been demonstrated con-
electrical properties. clusively [20].
In addition to the traditional optical and electrical devices, re- In this work, Sb2Se3 thin films were prepared and annealed in
sistance random access memory (RRAM) has received a great deal of flowing nitrogen ambient with different temperatures ranging from
attention owing to its high density, low power consumption, fast 150 °C to 450 °C. The effects of annealing temperature on the structure
switching speed, high scalability and multilevel storage [13,14]. The and optical properties of Sb2Se3 thin films were systematically in-
RRAM devices are suitable for new technological applications, vestigated. Moreover, a typical Sb2Se3-RRAM was also fabricated for

⁎
Corresponding author at: Department of Optical Science and Engineering, Fudan University, Shanghai 200433, China.
E-mail address: lijing@fudan.edu.cn (J. Li).

https://doi.org/10.1016/j.rinp.2019.102228
Received 10 December 2018; Received in revised form 21 March 2019; Accepted 21 March 2019
Available online 27 March 2019
2211-3797/ © 2019 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/BY-NC-ND/4.0/).
C. Liu, et al. Results in Physics 13 (2019) 102228

further characterizing the nature of memristive behaviors. The bipolar

memristive switching behavior as well as reversible switching property
were successfully observed in Ag/Sb2Se3/W heterojunction. All these
features render that Sb2Se3 is a promising semiconductor material for
integrated optical system and chalcogenide-based memory devices.

Experimental

Sample preparation

In terms of experiments, Sb2Se3 thin films were deposited on the

fused quartz substrates by radio-frequency (RF) magnetron sputtering
system at room temperature. The deposition power of the magnetron
loaded with a 99.99% purity Sb2Se3 target was fixed to 60 W, while the
sputtering time was set to 450 s. The background pressure of the
chamber and working pressure were approximately 7 × 10−6 mbar and
2.8 × 10−3 mbar, respectively. To obtain different degree of crystal-
lization, the samples were annealed at 150 °C, 250 °C, 350 °C and 450 °C
Fig. 1. XRD patterns of Sb2Se3 thin films annealed at different temperatures.
for 30 min in flowing nitrogen ambient. These five Sb2Se3 film samples
were named S1, S2, S3, S4, S5, corresponding to the as-deposited and
annealed films with successively increasing temperature. For fabri- samples also changes from (1 2 0) plane to (0 2 0) plane, which reveals
cating Sb2Se3-based metal-insulator-metal (MIM) structure, a 100 nm- the reduction in crystallinity.
thick W bottom electrode (BE) with was deposited on a SiO2 (300 nm)/ The mean grain sizes (D) can be calculated by Debye-Scherrer
Si substrate. Then the Sb2Se3 function layer with 450 s was deposited on equation,
the substrate. Next, in order to prevent Ag diffusion during annealing
0.9λ
process, the structure composed of functional layer and bottom elec- D=
β cosθ
trode (Sb2Se3/W) was annealed at 350 °C and then cooled down to
room temperature. At last, the Ag top electrode (TE) with Φ100 μm was where λ is the wavelength of X-ray radiation (1.54056 Å), β represents
deposited by a shadow mask assisted. the full width at half-maximum of the peak and θ refers to the angle of
Bragg diffraction. According to the XRD patterns, the calculated D and
Characterization methods the (1 2 0) interplanar spacing (d) of S3-S5 are listed in Table 1. The
significant decrease in the intensity of diffraction peaks of S5 may be
The structural characterizations of the thin films were investigated attributed to two possible reasons. On the one hand, the grain size and
by X-ray diffraction (XRD, Bruker D8 ADVANCE). The scanning range interplanar spacing are abnormally increased when the sample is an-
of diffraction angles was set from 10.0° to 60.0° with a step size of 0.02°. nealed at an excessively high annealing temperature. These changes
The optical transmittance spectra were characterized by using a double will decrease the film density and increase the surface roughness, thus
beam UV–VIS-NIR spectrophotometer (Shimadzu UV-3600). the film structure becomes loose. On the other hand, when the sample is
Spectroscopic ellipsometry (SE) was applied to determine the thick- annealed at an excessively high temperature, the defect concentrations
nesses and optical parameters of the samples via Drude−Lorentz model are increased owing to thermal diffusion or excessive evaporation of the
in the wavelength range of 350–800 nm. The thickness of Ag/Sb2Se3/W material. Therefore, the intensity of the diffraction peaks decreases.
sample was analyzed by scanning electron microscopy (SEM). The re- Similar results are reported in previous literature [22].
sistive switching characteristics of the heterostructure cells were mea-
sured by an Agilent B2912A semiconductor parameter analyzer. All the
electrical characteristics were measured by applying bias to the Ag TE Annealing effect on optical properties
while the W BE was ground.
Presented in Fig. 2 are the optical transmittance spectra measured in
Results and discussion the wavelength range of 380–2000 nm for Sb2Se3 thin films annealed at
different temperatures. Obviously, the transmittance of all samples in
Thickness fitting and structural analysis near-infrared light region is higher than that in visible light region. It
indicates that Sb2Se3 is an infrared transparent material, which can be
The thicknesses of S1-S5 determined by SE are 93.1 nm, 90.7 nm, applied to various integrated optical systems [23,24]. For simplicity,
88.7 nm, 86.5 nm and 73.5 nm, respectively. The film thickness de- the transmittance curves are divided into three groups, namely, G1, G2
ceases with increasing annealing temperature. Fig. 1 shows the XRD and G3. For G1, S1 and S2 are almost the same in both trend and value.
patterns of both as-deposited and annealed Sb2Se3 thin films. No dif- The maximum transmittance is nearly 100%. Similarly, the two curves
fraction peaks are observed for S1 and S2, implying their amorphous of G2 also show the same trend while the values of S4 are slightly
nature and the amorphous phase can be stabilized up to 150 °C. As the smaller. Comparing G1 and G2, the transmittance of the latter decreases
annealing temperature increases, sharp Bragg diffraction peaks are obviously in the whole spectra and the absorption edge of G2 shift to-
observed in S3-S5, which reveals that the prepared Sb2Se3 samples are wards longer wavelength (red-shift), indicating that the band gap
of the same orthorhombic phase and polycrystalline in nature (JCPDS
No: 015-0861) with unit cell parameters a, b, and c are 11.63, 11.78 Table 1
Mean grain size and (1 2 0) interplanar spacing of S3-S5.
and 3.98 Å, respectively. The same basic structure results are also re-
ported by Ref [21]. The intensity of the diffraction peaks increases as Sample D (nm) d (Å)
the annealing temperature increases from 250 °C to 350 °C, indicating
S3 41.83 5.2557
improvement of crystallinity for these samples. When the annealing
S4 48.09 5.2257
temperature is increased to 450 °C, the intensity of the diffraction peaks S5 77.97 5.2434
decreases significantly. In addition, the preferred orientation of the

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C. Liu, et al. Results in Physics 13 (2019) 102228

section, the curves also can be divided into three groups. Compared to
the amorphous phase of S1 and S2, the refractive index n and extinction
coefficient k of S3 and S4 are obviously increased. This is mainly be-
cause the unsaturated defects gradually decrease and grain sizes in-
crease during annealing process [27]. Additionally, the value of ex-
tinction coefficient k increases with the increase crystallinity of Sb2Se3.
It turns out that thermal treatment can improve photon absorption
capacity of the sample since the extinction coefficient k represents in-
terband transition of inside electron. For Sb2Se3 thin film annealed at
450 °C, the optical constants changes abnormally, corresponding to the
theory that most of chalcogenide materials no longer maintain their
optical properties when annealed at a higher temperature [28,29].
The optical band gap (Eg) of Sb2Se3 thin films can be determined
experimentally by the Tauc plot method [30],
αhν = A (hν − Eg )m

where α is the absorption coefficient which can be calculated by

Fig. 2. Transmittance spectra of Sb2Se3 thin films annealed at different tem- α = 4πκ / λ [31], hν is the incident photon energy, A is a constant which
peratures. related to effective mass and m is a constant that determines type of
optical transitions. For Sb2Se3, m is equal to 1/2 since it is a direct
allowed transition semiconductor material [32]. The fitted optical band
becomes narrow after thermal treatment. For G3, S5 presents different
gap of amorphous and crystalline Sb2Se3 are shown in Fig. 4. The op-
variation trend, i.e., the transmittance is the lowest of the five samples
tical band gap values are found to be 1.80 eV and 1.75 eV for amor-
and no significant interference can be observed. The possible reasons
phous phase, while it decreases to 1.50 eV when the sample is con-
may be associated with the increase of defects and the light scattering
verted to crystalline phase. Then the optical band gap is further
caused by an abnormal increase in grain size.
decreased to 1.40 eV as the annealing temperature increases to 450 °C.
The optical constants of Sb2Se3 thin films were measured by SE, a
Obviously, the band gap becomes narrower with the increase of the
precise nondestructive apparatus to fit optical parameters [25]. A three-
annealing temperature, corresponding to the red-shift of transmittance
layer model (ambient/film/substrate) was proposed to fit the ellipso-
spectra.
metric spectra according to the film structural properties. For the main
layer (Sb2Se3 thin film) with the best physical meaning, the Drude−-
Lorentz model is applied to fit the ellipsometric data. The model is Memristive switching behaviors
given by following expression [26],
Based on the above analysis results, S4 exhibits better crystalline
ωp2 Ck structure and optical properties. Therefore, the structure composed of
ε = ε∞ − + ∑ functional layer and bottom electrode (Sb2Se3/W) was also annealed at
ω2 + iωγ k
ωk2 − ω (ω + iγk )
350 °C in the process of preparing sample. Fig. 5(a) depicts the sche-
where ε∞ represents the dielectric response for nonatomic polarizations matic diagram of the Ag/Sb2Se3/W cell. The total thickness of the cells
at high light frequencies, γ is the plasmon damping constant of the is 273 nm and that of the Sb2Se3 layer is 84 nm, as shown in Fig. 5(b).
Drude part, ωp refers the unscreened plasma angular frequency, γk , ωk The typical switching characteristics of Ag/Sb2Se3/W cells with
and Ck indicate the damping factor, resonant frequency and strength compliance current of 100 mA are illustrated in Fig. 6(a), in which the
parameter of different oscillators, respectively. In the setting of para- arrows represent the sweeping directions. When a positive voltage
meters, the minimum wavelength, maximum wavelength and the sweep is applied to the Ag TE, the sample cell switches from the high-
number of oscillators are 350 nm, 800 nm and 3, respectively. In order resistance (HRS) to the low-resistance (LRS). In contrast, a negative
to obtain more accurate fitting results, all Sb2Se3 thin films are fitted at voltage sweep switches the sample cell from LRS to HRS. It is clear that
three light incident angles of 65°, 70° and 75°. the cell has bipolar resistive switching behavior with SET at a positive
The fitting results are shown in Fig. 3. It is clear that the values of sweep and RESET at negative sweep voltages. Besides, Fig. 6(b) por-
refractive index n and extinction coefficient k are relatively high in the trays the repetitive cycles I-V characteristics of the Ag/Sb2Se3/W cells.
whole visible light region. It means that Sb2Se3 is a kind of material It can be confirmed that the cells exhibit stable bipolar RS behavior
with high refraction and high absorption. As mentioned in the previous during the 100 cycles.

Fig. 3. (a) Refractive index n and (b) extinction coefficient curves k of the Sb2Se3 thin films annealed at different temperatures.

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C. Liu, et al. Results in Physics 13 (2019) 102228

Fig. 4. The optical band gaps of Sb2Se3 thin films annealed at different temperatures.

In order to understand the conduction mechanism of the Ag/ 9 με0 εr V 2

J=θ
Sb2Se3/W heterojunction, the I-V curves are replotted in a log(I)–log(V) 8 L3
scale, as shown in Fig. 7. Two different linearly fitting slope regions are
where θ is the ratio of free and trapped charge, ε0 is the permittivity of
observed in the positive sweeps in Fig. 7(a). The slope of the linear
free space, εr is the relative dielectric constant of the film, μ is the
proportion for current to voltage in LRS is roughly equal to 1, indicating
electron mobility, V is the voltage and L is the thickness of the film.
that the conductive law of LRS is Ohmic conduction (I ∝ V). This result
Based on the above analysis, the Ag/Sb2Se3/W heterostructure is a
is agreement with the conductive filament mechanism, that is, the
metal conductive filament resistance memory and the resistance effect
formation of conductive filaments connects the TE and BE. In HRS, the
is controlled by oxidation-reduction reaction. Previous reports on the
conduction mechanism is obviously different, namely, the slope of the
formation of conductive filament can support our speculation [34,35].
fitting curve is equal to 1 at low voltage, depicting an Ohmic conduc-
The process of the formation and rupture of Ag filaments can be de-
tion. The reason is that the density of thermally generated carriers is
scribed as follows. When the positive voltage is applied to the Ag TE,
large than that of injected carriers. As the applied voltage increases, the
the Ag atoms are oxidized to Ag ions as Ag → Ag+ + e− . Under the
fitting slope increases to 2, corresponding to the Child's square law
action of electric field, the Ag ions migrate to the W BE and they are
(I ∝ V2). The conductive characteristics of the HRS are consistent with
reduced to metallic Ag atoms as Ag+ + e− → Ag . Therefore, Ag fila-
the SCLC mechanism. When the applied voltage is low, there are no free
ments gradually grow from the W BE to Ag TE. These formed Ag con-
electrons in the film because the injected electrons are trapped in the
ductive filaments switched the device to the LRS. In contrast to the
traps. Therefore, the current is very low, i.e., the device is in HRS. Once
positive voltage, when a negative bias is applied to the Ag TE, the Ag
the traps are filled, the electrons flow into conduction band. Then the
atoms in the conductive filaments are oxidized to Ag ions once again.
Ag/Sb2Se3/W cell switches from HRS to LRS.
Thus, the Ag/Sb2Se3/W switches from LRS to HRS by rupturing the
There are also two different linearly fitting slope regions in the
conductive filaments.
negative sweeps, as depicted in Fig. 7(b). Within low voltage, the slope
value is roughly 1, exhibiting Ohmic conduction (I ∝ V). Then the
trapped carriers are being released from traps, so the slope shifts to 2, Conclusion
presenting SCLC. In the meantime, the Ag/Sb2Se3/W cell is in re-tran-
sition state from LRS to HRS. The current density in SCLC can be re- In summary, Sb2Se3 thin films have been successfully prepared
presented as [33], using RF magnetron sputtering method. Optical properties and resistive
switching behaviors in Sb2Se3 thin films with different annealing tem-
peratures and Ag/Sb2Se3/W heterojunctions were investigated

Fig. 5. (a) Schematic diagram and (b) cross sectional SEM image of Ag/Sb2Se3/W sample.

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C. Liu, et al. Results in Physics 13 (2019) 102228

Fig. 6. (a) Typical switching characteristics of Ag/Sb2Se3/W cells. (b) The I–V characteristic of Ag/Sb2Se3/W cells with certain number of sweep cycles.

defect states in polycrystalline Sb2Se3 thin film. Such excellent optical

properties as well as the characterization of resistive switching nature
render this a promising semiconductor material for integrated optical
system and chalcogenide-based memory devices.

Acknowledgments

The authors would like to express their sincere thanks for the fi-
nancial supports by the Natural Science Foundation of Shanghai, grant
numbers 17ZR1402200, and 13ZR1402600, National Natural Science
Foundation of China, grant numbers 60578047, and 61427815. The
authors would like to thank Professor Chen LY for his effective backup.

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