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Keywords: Dual-gate structure field-effect transistors (DG FETs) can provide various advantages such as high output cur-
Oxide nanowire rent, enhanced mobility, and tunability of threshold voltage (VTH) by adversely controlling the two channels
Dual-gate formed at both top and bottom gate dielectric interfaces. Here, we present high-mobility DG structure FETs using
Field-effect transistor crystalline Ga-doped In2O3 (IGO) nanowires (NWs) as channel and high-k ion-gel as a top gate dielectric layer.
Ga-doped In2O3
To enhance the electrical properties of IGO NW FETs such as field-effect mobility, on/off ratio, VTH, and sub-
Electrospinning
threshold slope, optimization of electrospinning, Ga doping in In2O3 NWs, and thermal annealing was carried
Ion gel gate dielectric
out. The optimized IGO NW FETs with a single SiO2 gate dielectric exhibited field-effect mobility of ~6.0 cm2/
(V·s), on/off ratio of > 107, subthreshold slope of 0.73 V/decade, and VTH of ~0 V. Also, the IGO NW FETs
showed excellent operation stabilities under positive-gate-bias and negative-bias-illumination stress conditions.
Furthermore, by using a high-k ion-gel film as the second gate dielectric layer, DG IGO NW FETs with field-effect
mobility up to ~35.1 cm2/(V·s) were realized which is comparably higher than those of single-gated IGO NW
FETs (6.0–6.5 cm2/(V·s)).
1. Introduction mobility of 20 cm2/(V·s) was demonstrated using SiO2 as the front and
back gate dielectric layers [5].
Recently, amorphous oxide semiconductor (AOS)-based field-effect In addition to the device structure modification, the utilization of
transistors (FETs) have attracted considerable attention in high-density crystalline oxide channel layers was also investigated. Here, instead of
active-matrix electronics owing to their high carrier mobility, good using amorphous oxide channel layer, highly crystalline oxide semi-
uniformity, and reasonable operation stability [1–4]. However, the re- conductors such as c-axis-aligned crystalline IGZO or polycrystalline
cent progress in high resolution, high speed, and low-power con- IGZO was employed as the channel layer. Owing to the highly crys-
sumption electronics has led to the development of FETs with superior talline structure and less defective states of the crystalline IGZO chan-
performance and stability overwhelming the conventional AOS FETs. In nels, FETs with improved mobilities and stabilities were realized [6].
this regard, several strategies have been devised to improve their per- Furthermore, oxide semiconductors with nanowire (NW) structures are
formances such as the crystallization of oxide channel layers, doping also of great interest as they can exhibit high electron mobilities and
with additional metallic atoms, and application of modified device ar- good electrical stability [7–17]. Previously, it was demonstrated that
chitectures. For example, dual-gate (DG) structure oxide FETs have crystalline oxide NWs such as ZnO and In2O3 NWs and their doped
been reported to enhance the mobility and stability, by utilizing the families could exhibit exceptionally high electron mobilities, out-
extended channel regions formed at both front and back interfaces and performing the single-crystalline Si-based FETs. For example, Ju et al.
by the reduced vertical electric field, respectively [5]. Here, by using reported pre-synthesized oxide NW FETs exhibiting a field-effect mo-
In–Ga–Zn–O (IGZO) as the channel layer, DG FETs having an apparent bility up to ~514 cm2/(V·s) [7]. Additionally, Zhou et al. demonstrated
⁎
Corresponding authors at: School of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon 16419, Republic of Korea (Y.-H. Kim).
School of Electrical and Electronics Engineering, Chung-Ang University, Seoul 06980, Republic of Korea (S.K. Park).
E-mail addresses: skpark@cau.ac.kr (S.K. Park), yhkim76@skku.edu (Y.-H. Kim).
1
These authors contributed equally to this work
https://doi.org/10.1016/j.apsusc.2020.145988
Received 23 December 2019; Received in revised form 28 February 2020; Accepted 5 March 2020
Available online 16 March 2020
0169-4332/ © 2020 Elsevier B.V. All rights reserved.
J. Kim, et al. Applied Surface Science 515 (2020) 145988
Fig. 1. (a) The fabrication of dual-gate (DG) IGO NW FETs using the electrospinning process. (b) In-plane SEM, and (c) a cross-sectional TEM images of IGO3 NWs
fabricated on a Si/SiO2 substrate. The topography and conductive atomic force microscope (AFM) images of (d) as-spun, and (e) 450 °C-annealed IGO3 NWs. In each
set, the left panel shows the topography image and the right panel shows the conductive AFM image.
In2O3 NW FETs having a field-effect mobility of 750 cm2/(V·s) which 2. Experimental Section
were fabricated by using the chemical vapor deposition (CVD) method
[8]. Even though these oxide NW FETs using pre-synthesized or CVD- 2.1. Preparation of metal-oxide precursor solutions for electrospinning
deposited oxide NW channels are noteworthy [8–10], the relatively
small deposition area, high process temperature, and rather low uni- For the fabrication of In2O3 and IGO NWs by electrospinning, cor-
formity can hinder their full utilization in large-area electronics. To responding precursor solutions were prepared by dissolving indium
resolve such issues, electrospinning method has been suggested to nitrate hydrate (In(NO3)3·xH2O) and gallium nitrate hydrate (Ga
fabricate the oxide semiconductor NWs since it can cover a relatively (NO3)3·xH2O) in N,N-dimethylformamide (DMF) (5 g). To increase the
large-area and provide high spatial uniformity [11–17]. For instance, viscosity of the solution appropriate for the electrospinning process,
Park et al. reported electrospun In2O3 NWs for the FET applications 0.7 g of polyvinylpyrrolidone (PVP, Mw ~1,300,000) was additionally
[13]. Here, by using ZrO2 as the passivation layer, In2O3 NW FETs dissolved in the solution. The precursor solution was then stirred for
having field-effect mobility of ~10 cm2/(V·s) were achieved. In addi- more than 24 h at room temperature before the electrospinning. All the
tion, various electrospun In2O3 NW FETs [9,12] and Gd-doped In2O3 metallic precursors, PVP and DMF were purchased from Sigma Aldrich
FETs [17] were also reported, demonstrating the feasibility of the and used without further modification. The total concentration of me-
electrospinning method for the formation of uniform oxide NW channel tallic precursors in the solution was fixed at 0.24 M, while the In:Ga
layer. Moreover, it was also reported that one-dimensional IGZO FETs molar ratio was varied as 10:0, 9:1, 8:2, 7:3 and 6:4. For simplicity,
can be fabricated on a polyimide wire substrate as a basic building IGOx is defined, representing the IGO NWs with an In:Ga molar ratio of
block for a flexible electronic textile system [18]. (10 – x):x (x = 0, 1, 2, 3 or 4).
In this study, to overcome the conventional thin-film type AOS FETs
and realize high-performance and high stability oxide-based FETs, DG
structure FETs having crystalline oxide NWs as the channel layer are 2.2. Electrospinning of In2O3 and IGO NWs and FET fabrication
demonstrated. Particularly, crystalline Ga-doped In2O3 (IGO) NW
channels are formed by using electrospinning and subsequent calcina- After the preparation of the precursor solutions, electrospinning of
tion process and utilized in DG FETs having a high-k ion gel film as the In2O3 and IGO NWs was carried out using an electrospinning/electro-
second top gate dielectric. Firstly, through the optimization of IGO NW spray machine (ESR200R2, NanoNC). As a substrate, we used a heavily
formation and Ga doping in the In2O3 matrix, IGO NW FETs with a doped p-type Si wafer with a 200 nm-thick SiO2 layer, where the Si
saturation field-effect mobility of ~6.0 cm2/(V·s), on/off ratio larger wafer and SiO2 layer served as the gate electrode and the gate dielectric
than 107, threshold voltage (VTH) of −0.8 ± 1.04 V, and subthreshold layer, respectively. During electrospinning, an electrical field of 13 kV
slope (SS) of 0.73 V/decade were obtained, with a single SiO2 gate was applied to eject the precursor solution from the syringe. The dis-
dielectric. The IGO NW FETs also exhibited excellent operation stabi- tance between the needle and substrate was set to 15 cm. After the
lities under positive-gate-bias stress (PBS) (ΔVTH = −1.17 V, at 5760 s) electrospinning of the solution, the sample was thermally annealed
and negative gate-bias illumination stress (NBIS) (ΔVTH = 0.30 V, at (calcined) at 150–450 °C for 2 h. Subsequently, the electrospun NW film
5760 s) conditions possibly due to the crystalline structure of the IGO was patterned by photolithography and wet etching. Then, aluminum
channel layer. Furthermore, by using a high-k ion gel film as the second (Al) source/drain electrodes with thickness of ~75 nm were deposited
top gate dielectric, DG oxide NW FETs were fabricated. The IGO NW DG by thermal evaporation and patterned using a metal shadow mask. The
FETs exhibited an improved apparent field-effect mobility of channel length (L) and width (W) of the FET were 100 and 1000 μm,
~35.1 cm2/(V·s) in an asymmetric operation, which is comparably respectively. Here, the channel width (W) is defined as the contact re-
higher than those of single-gate (SG) IGO NW FETs (6.0 cm2/(V·s) for gion made between the source or drain electrode and the patterned
SiO2 and 6.5 cm2/(V·s) for the ion-gel gate dielectric). We provide the oxide NW channel (Fig. 1(a)). To form an ion-gel gate dielectric for the
possible operation mechanisms for the IGO NW DG FETs under various DG FETs, an ion-gel solution consisting of poly(ethylene glycol) dia-
asymmetric operation modes. crylate (monomer), 2-hydroxy-2-methyl-propiophenone (photo-
initiator), and 1-ethyl-3-methylimidazolium bis
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J. Kim, et al. Applied Surface Science 515 (2020) 145988
Fig. 2. (a) In-plane SEM and microscope images of electrospun In2O3 NWs with different electrospinning time. (b) Optical images of fabricated In2O3 NW FETs. The
channel length and width of the FET were 100 and 1000 μm, respectively. (c) Transfer characteristics of single-gate (SG) In2O3 NW FETs with different electro-
spinning time. (d) Transfer characteristics of SG In2O3 NW FETs with different annealing temperature.
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J. Kim, et al. Applied Surface Science 515 (2020) 145988
the current, indicating that the NWs are electrically insulators. On the value was gradually increased for IGO3 and IGO4 NW FETs, having
other hand, after calcination, a clear contrast in the conductive AFM average VTH values of −0.8 ± 1.04 and + 7.2 ± 2.95 V, respectively
image was observed, which supports the claim that the NWs are elec- (Fig. 3(d)). The increase in on/off ratio and positive VTH shift are at-
trically activated and exhibit either semiconducting or conducting tributed to the suppression of oxygen vacancy formation by the Ga
characteristics. These microscopic analyses show that electrically doping and subsequent reduction in carrier concentration [20], in-
functioning oxide NWs can be fabricated by the electrospinning and dicating that the Ga plays a critical role in controlling the electrical
subsequent calcinations process. Additionally, during the calcination, properties of IGO NW FETs. In addition, the subthreshold character-
we observed a partial formation of welded junctions between the in- istics were also significantly improved by Ga doping as summarized in
dividual oxide NWs. Figs. S2a–2d in the ESM show the FESEM images of Table S1 in the ESM. While the In2O3 NW FET exhibited an SS value of
IGO3 and IGO4 NWs after calcination (450 °C). At the intersections 5.91 V/decade, the IGO3 and IGO4 NW FETs showed SS values of 0.73
between the NWs, physically welded junctions are formed. In parti- and 0.36 V/decade, respectively. The subthreshold characteristics are
cular, wider junctions and larger diameters of IGO4 NWs up to several closely related with the maximum density of interfacial trap states (Nt)
hundreds of nanometers were observed. It is expected that by the for- between the active channel layer and gate dielectric, by the following
mation of physically welded junctions between the oxide NWs, the equation [22],
carrier transport in the oxide NW channel can be promoted, as illu-
strated in Fig. S2e in the ESM, similar to that observed in silver-NW- SS × log(e ) C
Nt = ⎡ − 1⎤ i ,
based electrodes [19]. ⎢
⎣ kT / q ⎥
⎦q (1)
When the electrospun oxide NWs are used as the channel layer, the
areal density of oxide NWs and the annealing temperature are im- where k is the Boltzmann constant, q is the unit charge, and T is the
portant as the electrical properties of the transistors can be largely temperature. The Nt values of In2O3, IGO3, and IGO4 NW FETs were
governed by these factors. First, to optimize the areal density of oxide 1.06 × 1013, 1.22 × 1012, and 5.60 × 1011/(cm2·eV), respectively,
NWs for the channel layer, we varied the electrospinning time in the indicating that the density of interfacial trap states was significantly
range of 20–40 s. Here, we used In2O3 NWs as the reference material. reduced by the Ga doping. The field-effect mobility is another im-
Fig. 2(a) shows the in-plane SEM and optical microscopy images of the portant factor determining the performances of the FETs. As the mo-
In2O3 NWs electrospun for different times. As expected, a denser net- bility is related with the carrier concentration, it is likely that some
work was formed at the increased electrospinning time. Fig. 2(b) and degradation might occur upon the increase in Ga content in the In2O3
(c) show the fabricated In2O3 NW FETs and corresponding transfer (ID- NWs. Fig. 3(b) and (f) show the variation and distribution of field-effect
VG) characteristics, respectively (annealing temperature of 450 °C). mobility as a function of Ga concentration, respectively. The mobility
Although higher saturation mobility could be achieved with longer tends to decrease with the increase in Ga content, but the decrease was
electrospinning time (20 s: 9.3 cm2/(V·s); 30 s: 15.2 cm2/(V·s); 40 s: not substantial. For example, the average saturation mobilities of IGO3
19.9 cm2/(V·s)), a large negative VTH shift was simultaneously ob- and IGO4 FETs were 6.0 ± 0.63 and 3.1 ± 0.66 cm2/(V·s), respec-
served, which is detrimental for typical applications of FETs due to tively, which are slightly lower than that of the pristine In2O3 NW FETs.
depletion mode operation. Therefore, we set the electrospinning time to Furthermore, compared to that of the conventional film-type IGO3
~20 s in further experiments. Additionally, we investigated the effects FETs, the IGO3 NW FETs had reasonably high mobility (Fig. S3 in the
of the annealing temperature on the electrical properties of the In2O3 ESM). To conclude, upon the insertion of Ga into In2O3, although the
FETs. Fig. 2(d) shows the transfer characteristics of the In2O3 NW FETs field-effect mobility could be reduced to some extent, the improvements
annealed at different temperatures of 150 °C to 450 °C. Up to 250 °C, in on/off ratio, VTH, and subthreshold characteristics are substantial,
the FET showed negligible current modulation by the gate bias showing particularly for the IGO3 and IGO4 NW FETs.
that the channel layer is still in insulating states. This indicates in- In oxide FETs, light-induced instability is one of the critical issues
sufficient sol-gel reaction for the oxide formation and/or removal of the affecting their operational stabilities, which possibly originates from
PVP component. When the annealing temperature is increased equal or the deep states in the bandgap [23]. To investigate the light-induced
higher than 350 °C, the overall current density is increased with a clear instability of the oxide NW FETs, IGO3 and IGO4 NW FETs were sub-
modulation of drain current by the gate bias. The results show that jected to an NBIS test. Figs. 4(a) and S4a in the ESM show the variation
annealing temperature typically higher than 350 °C is required for the in VTH and transfer curves under the NBIS for stress times up to 5760 s,
formation of semiconducting In2O3 NWs using the current precursor respectively (VGS = −30 V, light power intensity = 0.85 mW/cm2).
system. Relatively good stabilities with ΔVTH of +0.30 V and +2.54 V were
Despite the reasonably high mobility of the In2O3 NW FETs, the observed in IGO3 and IGO4 NW FETs at a stress time of 5760 s, re-
relatively low current on/off ratio (~102) can hinder its practical ap- spectively. The stable operation under the NBIS can be attributed to the
plications in active-matrix electronics. Because the low on/off ratio is reduced light absorption area of the IGO NW channel compared to that
typically related to the high carrier concentration of the channel layer, of the film-type channel layer. The effective channel area of IGO3 NWs
we adopted a carrier suppressor to control the carrier concentration covering the surface was approximately 14.4%, as shown in Fig. S5 in
[20]. Here, we added Ga in the In2O3 NWs which has high Gibbs energy the ESM. Also, the stabilities under the PBS were evaluated. Figs. 4(b)
of oxidation (−661 kJ/mol) [21]. Fig. 3(a) and (e) show the transfer and S4b in the ESM show the variations in VTH and transfer curves
and output characteristics of In2O3 and Ga-doped In2O3 (IGO) NW FETs under PBS (VGS = +30 V) condition, respectively. The IGO3 and IGO4
with different Ga concentrations (IGO1, IGO2, IGO3, and IGO4), re- NW FETs exhibited ΔVTH of −1.17 V and +0.10 V at the stress time of
spectively, fabricated with the annealing temperature of 450 °C. Also, 5760 s, respectively, showing that the IGO NW FETs are relatively
Fig. 3(b)–(d) show the saturation field-effect mobility, current on/off stable under the continuous bias conditions.
ratio, and VTH as a function of Ga concentration, respectively. Afore- Using the optimized oxide NW channel layer, DG NW FETs were
mentioned, the In2O3 NW FET exhibited a relatively high mobility fabricated by forming a high-k ion-gel film as the top gate dielectric
(8.2 ± 1.33 cm2/(V·s)). However, the off-state current level was higher layer. One of the key aspects of using the ion-gel dielectric is the low-
than 10−6 A, which led to a low on/off ratio (102–103). Moreover, VTH voltage operation due to its high dielectric constant [24]. In addition,
was considerably negative (−14.9 ± 3.62 V), indicating a deep-de- owing to its simple fabrication and room-temperature processability,
pletion-mode operation. Upon the increase in Ga concentration, the on/ the DG NW FETs can be easily realized by simply forming the ion-gel
off ratio and VTH considerably changed. As shown in Fig. 3(c), the on/ film on top of the oxide NW channel layer. Fig. 5(a) shows the sche-
off ratio exhibited a steep increase up to 107–108 when the Ga con- matic device structure and an optical image of DG IGO3 NW FETs. Prior
centration was higher than 30% (IGO3 and IGO4). Moreover, the VTH to the DG operation, we analyzed the electrical characteristics of the
4
J. Kim, et al. Applied Surface Science 515 (2020) 145988
Fig. 3. (a) Transfer characteristics of SG In2O3 and IGO NW FETs with different Ga concentrations. The variations of (b) saturation field-effect mobility, (c) current
on/off ratio, and (d) VTH as a function of Ga concentration. (e) Output curves of SG In2O3 and IGO NW FETs with different Ga concentrations. (f) Statistical data of
saturation field-effect mobility of SG In2O3 and IGO NW FETs.
5
J. Kim, et al. Applied Surface Science 515 (2020) 145988
Fig. 5. (a) A schematic device structure and an optical microscope image of a DG IGO3 NW FET using an EMIM:TFSI ion-gel film as the top gate dielectric. (b) Areal
capacitance-voltage data of the ion-gel gate dielectric film measured at 100 Hz. (c) Transfer characteristics of ion-gel-gated IGO3 NW FETs (single gate mode,
VD = 2 V). The grey color line shows the gate leakage current (IG) of the device. (d) Statistical data of field-effect mobility, VTH, and subthreshold slope (SS) of ion-
gel-gated IGO3 NW FETs.
6
J. Kim, et al. Applied Surface Science 515 (2020) 145988
Fig. 6. (a) Transfer characteristics of DG IGO3 NW FETs when the bottom gate bias (VG1) was swept in the range of −30 V ~ +30 V at different top gate biases
(VG2 = −2, −1, 0, 1, 2 V). (b) The variation of VTH as a function of VG2 bias. The VTH values are obtained in both forward (−30 V → +30 V) and reverse (+30 V →
−30 V) sweep conditions. (c) Corresponding operation mechanism of the DG IGO3 NW FETs (VG1 forward sweep). (d) Transfer characteristics of DG IGO3 NW FETs
when the top gate bias (VG2) was swept in the range of −2 V ~ +2 V at different bottom gate biases (VG1 = −30, −15, 0, 15, 30 V). (e) The variation of VTH as a
function of VG2 bias. The VTH values are obtained in both forward (−2 V → +2 V) and reverse (+2 V → −2 V) sweep conditions. (f) Corresponding operation
mechanism of the DG IGO3 NW FETs (VG2 sweep).
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supported by the National Research Foundation (NRF) of Korea, grant- [5] M. Nag, H. Celiker, L. Verschueren, S. Smout, M. Willegems, R. Upadhyay, C. Rolin,
funded by the Korea Government (Ministry of Science and ICT; NRF- N. Papadopoulos, J. Genoe, W. Dehaene, S. Steudel, P. Heremans, K. Myny, P-12:
High performance dual-gate dual-layer amorphous oxide semiconductors TFTs on
2017R1E1A1A01077189, NRF‐2019M3F3A1A02071601 and NRF- PI foil for display application, SID Symp. Dig. Tech. Pap. 50 (2019) 1255–1258,
2019R1A2C2002447). https://doi.org/10.1002/sdtp.13161.
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