Chemical Physics Letters 742 (2020) 137174

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Chemical Physics Letters

journal homepage: www.elsevier.com/locate/cplett

Research paper

Controllable phase transition ITO nano powders and temperature-structure T

sensitivity
⁎
Xiaoyu Zhaia, Yiqing Zhanga,b, Yujie Chena, Yunqian Maa, Jiaxiang Liua,
a
Beijing Key Laboratory of Electrochemical Process and Technology for Materials, College of Materials Science and Engineering, Beijing University of Chemical Technology,
Beijing 100029, China
b
Mechanical and Electronic Engineering Department, Henan Polytechnic, Zhengzhou 450046, China

H I GH L IG H T S

• Preparing flexibly controllable phase transition ITO NPs by hydrothermal method.

• Fabricating 150 nm single cubic phase and 20 nm single hexagonal phase ITO NPs.
• Deeply revealing the phase transition relationship between precursors and oxides.

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

Keywords: Flexibly controllable phase transition indium tin oxide (ITO) nano powders (NPs) were prepared by an en-
Hydrothermal method vironmentally friendly hydrothermal method. The characterization results show that ITO NPs undergo a novel
Phase transition phase transition from cubic phase to hexagonal phase with hydrothermal temperature increasing. Single cubic
Hexagonal indium tin oxide nano powders and hexagonal phase ITO NPs with a diameter of 150 and 20 nm were respectively synthesized at 120 and 250 ℃
Fluorescence
hydrothermal temperature combined with a followed 550 ℃ calcination process. The fluorescence emission
Temperature-structure sensitivity
intensity of hexagonal ITO (h-ITO) NPs was stronger than the one of cubic ITO (c-ITO) NPs due to more oxygen
vacancies.

1. Introduction Gao et al. [11] have got InOOH in In(NO3)3/ethylene glycol/ethanol/

Transparent conductive indium tin oxide (ITO) is widely used in
optoelectronic devices, such as liquid crystal flat panel display, thin
film transistor and transparent electrode/substrate material [1–4], due
to its high electrical conductivity, transparency to light and infrared
reflectivity [5–7]. There are two different crystal structures of ITO,
containing cubic phase and hexagonal phase. Cubic ITO (c-ITO) is a
normal temperature and pressure phase, showing the same structure of
Fe-Mn ore. However, hexagonal ITO (h-ITO) is a high temperature
(> 800 ℃) and pressure (103-107 kPa) phase, showing the same
structure of corundum. Due to the better anion layer filling structure in
h-ITO, h-ITO shows some advantages compared to c-ITO, such as higher
specific gravity, higher green density and more stable conductivity [8].
In addition, h-ITO shows many excellent properties such as high
ethanol sensitivity [9] and high catalytic activity [10].
Owing to that the presence of water is bad for the preparation of h-
ITO [11], most of the researches have been focused on synthesizing h-
ITO by solvothermal method or water-solvent binary system, currently.
NaOH system and obtained h-In2O3 by calcining at 500 ℃ for 2 h based
on solvothermal method. Tao et al. [12] have acquired InOOH in
ethylene glycol/water/urea system and obtained h-In2O3 by calcining
at 400 ℃ for 2 h based on solvothermal method. Moreover, Liu et al.
[13] have prepared h-In2O3 in acetyl acetone indium/methanol/water/
ethanol system at 200 ℃ for 48 h by a hydrothermal method. However,
the above methods have the same shortcomings due to the use of or-
ganic solvent or indium tin organic salt, such as strong toxicity, high
cost and certain risk during the operation process. Thus, setting up an
effective, low cost and environmentally friendly way, such as hydro-
thermal method without organic solvent and indium tin organic salt, to
prepare h-ITO, is a prerequisite for developing high-performance op-
toelectronic components. Moreover, process variables will also have
important influences on the morphology and properties of ITO powders
[14].
In this paper, using metal In and SnCl4·5H2O as the raw materials,
urea as precipitant, InOOH precursor was prepared by hydrothermal
method and then h-ITO was obtained by calcining the precursor at

⁎
Corresponding author.
E-mail address: ljxpost@263.net (J. Liu).

https://doi.org/10.1016/j.cplett.2020.137174
Received 20 November 2019; Received in revised form 17 January 2020; Accepted 1 February 2020
Available online 01 February 2020
0009-2614/ © 2020 Elsevier B.V. All rights reserved.
X. Zhai, et al. Chemical Physics Letters 742 (2020) 137174

550 ℃ for 3 h. The influences from reaction temperature on the crystal

structure, morphology and optical properties of ITO powders, prepared
by hydrothermal growth technology, were studied systematically.
Without any organic solvents, h-ITO nano powders (NPs) with good
crystallinity were prepared. By tuning the hydrothermal temperature,
the crystal phase transition can be easily controlled from cubic phase to
hexagonal phase. This paper provides a new effective way, hydro-
thermal method, to prepare h-ITO NPs. Significantly, this method
possesses several advantages, including low cost, non-toxic, en-
vironmentally friendly and simple preparation process.

2. Experimental

2.1. Reagents

HNO3 (GR) was purchased from Beijing Tong Guang Fine Chemicals Fig. 1. XRD patterns of precursors prepared at different hydrothermal tem-
Company. Metal In (purity: 99.99%) was purchased from Liuzhou peratures.
Smelting Company. Urea (GR) and SnCl4·5H2O (mass ratio: 99.99%)
were purchased from Sinopharm Chemical Regent Beijing Co., Ltd. All
reagents were used as received.

2.2. Preparation of ITO NPs

3 g indium was dissolved in concentrated nitric acid under vigorous

stirring and heating at 60 ℃ to prepare In(NO3)3. In(NO3)3 solution was
mixed with SnCl4·5H2O with the In2O3/SnO2 mass ratio of 9:1. Urea
solution, prepared with a certain amount of urea (n (In3+): n
(urea) = 1:5), was added into the above mixed solution. After being
stirred for 0.5 h, the suspensions were transferred into teflon-lined
stainless steel autoclaves and heated at different reaction temperatures
(120, 160, 200, 240 and 250 ℃) for 6 h. The precipitates were washed
by deionized water and absolute ethanol to remove chloride ions and
nitrate ions and dried at room temperature for 12 h. The precursors
were finally calcined at 550 ℃ for 3 h to prepare yellow ITO NPs.
Fig. 2. XRD patterns of ITO powders prepared at different hydrothermal tem-
peratures with calcining at 550 ℃.
2.3. Characterization

TG curves were recorded using a DTG-60A thermal analysis system
with a heating rate of 10 ℃/min. Powder X-ray diffraction patterns
(XRD) were recorded using a Rigaku D/Max-2400 diffractometer with
Cu Kα radiation (1.5418 Å). Raman spectra were recorded using a
Renishaw InVia confocal microprobe Raman system. Morphologies
were recorded using a H-800 transmission electron microscopy (TEM).
Solid-state fluorescence emission spectra were recorded on a Hitachi F-
7000 FL spectrophotometer. X-ray photoelectron spectroscopy (XPS)
curves were recorded on a Thermo Fisher Scientific ESCALAB 250
system.
3. Results and discussion
3.1. Structural study on precursors and ITO NPs
XRD pattern can help to analyze the structure of a crystal [15].
Fig. 1 shows the XRD patterns of precursors prepared at different hy-
drothermal temperatures. As shown in Fig. 1, the In(OH)3 precursors
eventually transformed into InOOH with the increase of hydrothermal
temperature. When the reaction temperature was 120 ℃, the products
showed cubic In(OH)3 phase (JCPDS No. 76-1463). When the reaction
temperature was 200 ℃, the products consisted of two crystal phases,
orthorhombic InOOH phase (JCPDS No. 71-2283) and cubic In(OH)3
phase (JCPDS No. 76–1463). However, the XRD pattern was in good
agreement with orthorhombic InOOH phase (JCPDS No. 71-2283) at
250 ℃, indicating the successful preparation of orthorhombic InOOH
phase precursors.
The precursors were calcined at 550 ℃ for 3 h to prepare ITO
powders. Fig. 2 shows the XRD patterns of ITO powders prepared at
different hydrothermal temperatures. The crystal structure of ITO
powders transformed from cubic phase to hexagonal phase with the
increase of reaction temperature, corresponding to the precursor’s
transition from In(OH)3 to InOOH. When the hydrothermal temperature
was 120 ℃, the product showed cubic In2O3 phase (JCPDS No. 71-
2194), proving the successful synthesis of c-ITO. However, when the
hydrothermal temperature was 250 ℃, the product showed hexagonal
In2O3 phase (JCPDS No. 22-0336), meaning the successful synthesis of
h-ITO. Moreover, when the hydrothermal temperature was between
120 and 250 ℃, the XRD pattern showed two phases of cubic In2O3
structure (JCPDS No.71-2194) and hexagonal In2O3 structure (JCPDS
No.22-0336). Combining with the result shown in Fig. 1, it can be
proved that the structure of precursor plays a key role in the structure of
oxide. The corresponding relationship between indium-tin hydroxide
and oxide is agreement with previous references [16,17]. In the hy-
drothermal reaction, a large number of OH– generated due to the de-
composition of urea, making In3+ hydrolysis to form In(OH)3. With
increasing reaction temperature, the obtained In(OH)3 nuclei elimi-
nated water molecules from their core to form InOOH [18]. Cubic In2O3
could be obtained by thermal dehydration of In(OH)3, while hexagonal
In2O3 was prepared by thermal dehydration of InOOH. The reactions
during this process could be expressed as follows:
CO(NH2)2+3H2O → 2NH4++2OH–+CO2↑ (1)
In3++3OH– → In(OH)3 (2)
In(OH)3 → InOOH + H2O (3)
2In(OH)3 → c-In2O3 + 3H2O (4)

2
X. Zhai, et al.
Fig. 3. TG curves of the precursors prepared at different hydrothermal tem-
peratures.
2InOOH → h-In2O3 + H2O (5)
TG analysis was used to examine the conversion process of pre-
cursors during calcination. Fig. 3 shows the TG curves of precursors
prepared at different hydrothermal temperatures. The total mass losses
of three precursors were 19.07%, 9.4% and 8.11% (25 to 800 ℃) when
the reaction temperatures were 120 ℃, 200 ℃ and 250 ℃, respectively.
The TG curves could be divided into three stages. In the first stage, from
25 to 200 ℃, the mass loss was caused by the removal of adsorbed
water and glycol in the precursors. The second stage is from 200 to
550 ℃ and the mass loss was caused by the thermal dehydration from
precursor to oxide. The theoretical mass loss caused by the phase
transition from In(OH)3 to c-ITO and InOOH to h-ITO were 16.28% and
6.09%, respectively. For the precursors obtained at 120 and 250 ℃, the
mass losses caused by the phase transition from In(OH)3 to c-ITO and
InOOH to h-ITO were 16.88% and 5.92%, respectively. The experi-
mental mass losses were very close to the theoretical mass losses. For
the precursor prepared at 200 ℃, the mass loss of 8.54% for the second
stage was between the two theoretical values due to the precursor
consisted of In(OH)3 and InOOH. With increasing hydrothermal tem-
perature, the mass loss in the second stage decreased, indicating the
increase of the amount of InOOH phase, which is in consistent with the
XRD analysis. In the third stage from 550 to 800 ℃, TG curves tended to
be horizontal lines, which meant that ITO phase fully formed when the
calcination temperature was above 550 ℃.
In order to study the effect of temperature on phase transition,
Raman spectra were recorded. Fig. 4 shows the Raman spectra of ITO
powders prepared at different hydrothermal temperatures. For c-In2O3,
the optical vibration modes are shown below [19]:
Fig. 4. Raman spectra of ITO powders prepared at different hydrothermal
temperatures.
3
Chemical Physics Letters 742 (2020) 137174
Γopt = 4Ag + 4Eg + 14Tg + 5Au + 5Eu + 16Tu (6)
Ag, Eg and Tg represent the Raman active vibration modes. Au and Eu
represent inactive modes. Tu represents infrared active vibration mode.
Fig. 4 shows the Raman vibrational modes, located at 132, 306, 365,
495 and 627 cm−1, respectively, which are in good agreement with the
ones of c-In2O3 [20]. This result proved that c-ITO could be obtained at
120 ℃ after calcining at 550 ℃. For h-ITO, the optical vibration modes
are shown below [19]:
Γopt = 2A1g + 5Eg + 2A1u + 2A2u + 3A2g + 4Eu (7)
A1u, A2u, A2g and Eu are Raman active or infrared active vibration
modes. A1g and Eg are Raman active vibration modes. Fig. 4 shows the
Raman vibrational modes, located at 163, 219, 269, 305, 384, 501 and
590 cm−1, respectively, which are in good agreement with the ones of
h-In2O3 [21]. This also testified that h-ITO could be prepared at 250 ℃
after calcination at 550 ℃. However, ITO NPs prepared at 160 ℃ and
240 ℃ both show two kinds of vibrational modes. Significantly, the
Raman spectra of h-ITO and c-ITO were similar to the ones of h-In2O3
and c-In2O3 due to the main contribution to the vibrational modes
coming from the host lattice of h-In2O3 and c-In2O3. Novel phase
transition between cubic phase and hexagonal phase controlled by
hydrothermal temperature shows the excellent temperature-structure
sensitivity, meaning a potential application of temperature-structure
sensor.
3.2. Morphology of ITO NPs
TEM images were recorded to give microstructures [22] of ITO NPs
prepared at different hydrothermal temperatures. ITO NPs have been
prepared and studied by some scholars. However, fabricating ITO
submicron particles remains a challenge and has gained little attention
[23]. Fig. 5 shows the TEM images of ITO powders prepared at different
hydrothermal temperatures. When the reaction temperature was
120 ℃, the ITO NPs showed cubic shape with a particle size of 150 nm.
Continuing to increase the hydrothermal temperature to 160 ℃, ITO
NPs showed irregularly cuboid morphology. Moreover, when the re-
action temperatures were 200, 240 and 250 ℃, ITO NPs transformed
from cuboid to sphere and the particle sizes were 15, 18 and 20 nm,
respectively. When the hydrothermal temperature increased from 120
to 200 ℃, the particle size of ITO powders reduced dramatically. High
reaction temperature promoted the decomposition of urea and made
the pressure in the reaction still rise. Therefore, larger particles col-
lapsed to form small particles. An increased nucleation rate caused
more fine grains to generate due to the increased solubility of reactants.
And the solution reached a state of oversaturation at 200 ℃. According
to Ostwald ripening theory, the newly generated grains in the super-
saturated system began to grow up. The particles showed an increased
size due to continuous growth with the increase of hydrothermal tem-
perature. Significantly, particle size can be flexibly controllable by
tuning the hydrothermal temperature.
3.3. Fluorescence of ITO NPs
Fluorescence plays an important role in the research of semi-
conductor luminescence. At room temperature, bulk In2O3 material is
nonluminous matter [24]. However, nano-In2O3 shows light phenom-
enon due to oxygen vacancy and quantum confined effect.
Fig. 6 shows fluorescence emission spectra of h-ITO and c-ITO under
the same excitation wavelength at room temperature. The emission
spectra of h-ITO and c-ITO were similar and showed six emission peaks
at 411, 424, 450, 470, 483 and 492 nm in blue light region. H-ITO
showed higher fluorescence emission intensity than the one of c-ITO.
ITO shows a similar mechanism of blue light emission with In2O3. The
fluorescence emission peaks were not caused by quantum confinement
effect due to the large diameter, which is much larger than indium
X. Zhai, et al.
Fig. 5. TEM images of ITO powders prepared at different hydrothermal temperatures: (a) 120 ℃, (b) 160 ℃, (c) 200 ℃, (d) 240 ℃ and (e) 250 ℃.
Fig. 6. Fluorescence emission spectra of h-ITO and c-ITO NPs.
trioxide’s critical Bohr radius of 2.14 nm [25]. Besides oxygen vacancy,
the luminescence mechanism was also related to the tin ion doping
concentration. Maintaining tin dopant content constant in the experi-
ments, the probability of capturing electrons to make acceptor vacancy
form exciton increased when oxygen vacancy concentration increased.
Thereby, the probability of exciton radiative recombination increased
[26], which was shown in Equation (8) [27]. Ultimately, the photon
emission number of products increased, which was shown as an in-
creased luminescence intensity.
V ·o + (VIn ′Vo) ′ + hν → (VIn ′Vo) x + (Vo) x
The blue light emission intensity of h-ITO was stronger than the one
of c-ITO, which might be a result of more oxygen vacancies in h-ITO.
Fig. 7 shows the XPS spectra of two ITO NPs and the corresponding O1s
XPS spectra. According to Fig. 7a and c, two ITO NPs were both con-
sisted of In, O and Sn without other impurities, corresponding to the
XRD results. Fig. 7b and d show the O1s XPS spectra of c-ITO and h-ITO.
There were three separate peaks at 529.9, 531.1 and 531.7 eV, corre-
sponding to the oxygen of In-O, the oxygen of Sn-O and the oxygen of
In-O in a defective state, respectively [28]. The oxygen vacancy content
of O1s spectrum in c-ITO lattice was 17.534%. However, the oxygen
vacancy content of O1s spectrum in h-ITO lattice was 36.373%.
Chemical Physics Letters 742 (2020) 137174
Compared with c-ITO, h-ITO showed more oxygen vacancies. Sig-
nificantly, Fig. 6 showed that the blue light emission intensity of h-ITO
was stronger than the one of c-ITO. This phenomenon proved that
stronger blue light emission intensity was caused by more oxygen va-
cancies.
4. Conclusions
Controllable phase transition ITO NPs were prepared by hydro-
thermal method without organic solvent, showing several advantages,
such as green environment protection, simpler synthetic process, lower
cost and nonhazardous. ITO NPs undergo a controllable phase transi-
tion from cubic phase to hexagonal phase with the increase of hydro-
thermal temperature. Single cubic phase and hexagonal phase ITO NPs
with a diameter of 150 nm and 20 nm were respectively synthesized at
120 ℃ and 250 ℃ hydrothermal temperature combined with a followed
550 ℃ calcination process. The fluorescence emission intensity of h-ITO
NPs was stronger than the one of c-ITO NPs due to more oxygen va-
cancies. Hydrothermal temperature plays a key role in the structure,
morphology and optical properties of ITO NPs. Novel phase transition
between cubic phase and hexagonal phase controlled by hydrothermal
temperature shows the excellent temperature-structure sensitivity.
Significantly, this work not only deeply reveals the relationship be-
tween the transition of precursors and the phase transition of ITO NPs,
but also clarifies the effects from hydrothermal temperature on the
phase structure, morphology and fluorescence of ITO NPs, which will
promote the further research and wider application of next generation
(8) of ITO functional materials, such as temperature-structure sensor.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
Acknowledgments
This work was financially supported by Beijing Natural Science
Foundation (Grant No. 2192041).
4
X. Zhai, et al. Chemical Physics Letters 742 (2020) 137174

Fig. 7. XPS spectra of ITO NPs: (a) XPS spectra of c-ITO, (b) O1s XPS spectra of c-ITO, (c) XPS spectra of h-ITO and (d) O1s XPS spectra of h-ITO.

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