Systematic investigation of the growth

kinetics of β-Ga2O3 epilayer by plasma

enhanced chemical vapor deposition
Cite as: Appl. Phys. Lett. 116, 072102 (2020); https://doi.org/10.1063/1.5142196
Submitted: 10 December 2019 • Accepted: 09 February 2020 • Published Online: 19 February 2020

C. Wu, D. Y. Guo, L. Y. Zhang, et al.

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 Applied Physics Letters ARTICLE scitation.org/journal/apl

Systematic investigation of the growth kinetics

of b-Ga2O3 epilayer by plasma enhanced
chemical vapor deposition
Cite as: Appl. Phys. Lett. 116, 072102 (2020); doi: 10.1063/1.5142196
Submitted: 10 December 2019 . Accepted: 9 February 2020 .
Published Online: 19 February 2020

C. Wu,1 D. Y. Guo,1,2,a) L. Y. Zhang,1 P. G. Li,3 F. B. Zhang,4 C. K. Tan,5 S. L. Wang,1 A. P. Liu,1 F. M. Wu,1,a)

and W. H. Tang3

AFFILIATIONS
1
Center for Optoelectronics Materials and Devices and Key Laboratory of Optical Field Manipulation of Zhejiang Province,
Department of Physics, Zhejiang Sci-Tech University, Hangzhou 310018, China
2
State Key Lab of Silicon Materials, Zhejiang University, Hangzhou 310027, China
3
State Key Laboratory of Information Photonics and Optical Communications and Laboratory of Information Functional Materials
and Devices, School of Science, Beijing University of Posts and Telecommunications, Beijing 100876, China
4
Guangxi Key Laboratory of Precision Navigation Technology and Application, Guilin University of Electronic Technology,
Guilin 541004, China
5
Department of Electrical and Computer Engineering, Clarkson University, Potsdam, New York 13699, USA

a)
Authors to whom correspondence should be addressed: dyguo@zstu.edu.cn and wfm@zstu.edu.cn

ABSTRACT
b-Ga2O3 has attracted much attention due to its ultrawide-bandgap (4.9 eV) with a high breakdown field (8 MV/cm) and good thermal/
chemical stability. In order for b-Ga2O3 to be used in electronic and optoelectronic devices, epitaxial growth technology of thin films should
be given priority. However, challenges are associated with the trade-off growth rate with crystallization and surface roughness in conven-
tional epitaxy. Herein, plasma enhanced chemical vapor deposition was used to grow the b-Ga2O3 epilayer, and the growth kinetics process
has been systematically investigated. A high growth rate of 0.58 lm/h and a single ð201Þ plane orientation with a full width at half maxi-
mum value of 0.86 were obtained when grown on the c-plane sapphire substrate at the growth temperature of 820  C. Then, a proposed
model for the mechanism of nucleation and growth of b-Ga2O3 epitaxial films is established to understand the precursor transport and
gas phase reaction process. This work provides a cheap, green, and efficient epitaxial growth method, which is indispensable for device
applications of b-Ga2O3.
Published under license by AIP Publishing. https://doi.org/10.1063/1.5142196

In recent years, gallium oxide (Ga2O3) semiconductor has emerged
as a highly promising candidate for next generation power electronics
technology, attributed to its possession of an ultrawide bandgap energy of
4.9 eV. Owing to its possibility of replacing silicon-based substrates as the
next go-to substrate, Ga2O3 semiconductor also attracts much attention
in applications such as optoelectronics, memory, sensing systems, deep
ultraviolet transparent conductive oxide electrodes, and photocatalysts.1–4
Among the six known polymorphs of Ga2O3, known as a, b, c, d, e,
and j, the b-phase (monoclinic) is the most stable.5 In general, b-Ga2O3
semiconductor materials are thermally and chemically stable, exhibiting
decent electron mobility (100 cm2/V s) and high breakdown field
(8 MV/cm), which are comparable to other wide and ultrawide bandgap
semiconductor materials including SiC, AlN, and GaN.6
The development of epitaxial growth techniques is crucial in pro-
ducing high quality b-Ga2O3 thin films. The growth of the b-Ga2O3
epilayer has been conducted by various epitaxial growth techniques
including molecular beam epitaxy (MBE), halide vapor phase epitaxy
(HVPE), metal organic chemical vapor deposition (MOCVD), pulsed
laser deposition (PLD), and low pressure chemical vapor deposition
(LPCVD).7–10 However, challenges have been associated with the
trade-off between the growth rate and crystallization in conventional
epitaxial techniques. For example, the conventional epitaxial techni-
ques, MOCVD, PLD, and MBE, produce high quality Ga2O3 thin
films, but the low growth rate is not conducive to industrialization. On
the other hand, HVPE has the advantage of higher growth rate, but
the Ga2O3 epitaxial films exhibit a rough surface morphology that is

Appl. Phys. Lett. 116, 072102 (2020); doi: 10.1063/1.5142196 116, 072102-1
Published under license by AIP Publishing
 Applied Physics Letters
unsuitable for device processing. As a result, there is a strong need to
develop an epitaxial technique that provides reasonably high crystal-
line quality with a desirable growth rate.
Plasma enhanced chemical vapor deposition (PECVD) is one of
the well-established CVD techniques used in industry and research
due to its popularity in depositing insulating oxides for silicon-based
structures. PECVD offers numerous advantages such as low cost, low
deposition temperature, high reproducibility and scalability, high
deposition rate, and good uniformity of film thickness.11 While
PECVD appears to be a suitable method for the epitaxy of b-Ga2O3
thin films, surprisingly, there has been no relevant literature reported
up to present. Thus, demonstrating the feasibility of PECVD use in
synthesizing b-Ga2O3 thin films is an important step toward gauging
its potential as an epitaxial technique, which overcomes challenges
associated with other conventional methods.
In this work, b-Ga2O3 thin films were grown on c-plane sapphire
substrates by PECVD. The c-plane sapphire substrates with a 0
off-axis angle were purchased from TDG Holding Co., Ltd. Effects of
various growth parameters on the growth rate and crystallinity were
investigated systematically to determine the suitable growth condition
for the gallium oxide film. Our findings reveal that the growth rate of
the b-Ga2O3 epilayer for PECVD reaches 0.58 lm per hour, which
is higher than that of the MOCVD, MBE, and PLD techniques. In
addition, the b-Ga2O3 epilayer exhibits a single ð201Þ plane orienta-
tion with a full width at half maximum (FWHM) value of 0.86
through optimizations of the experimental parameters.
The PECVD system for epitaxial growth is shown in Fig. 1. High
purity metallic gallium (Ga) and oxygen gas (O2) were used as source
materials, and argon (Ar) was used as carrier gas. The prepared sap-
phire substrate was inverted in a quartz boat, which was placed at the
center of the furnace. The Ga source was first placed horizontally at
the upstream of the quartz tube. Then, the furnace was heated to the
reaction temperature of 820  C. O2 was then passed into the tube, and
the RF power source was turned on right afterwards. After 90 min of
reaction, the chamber was cooled to ambient temperature under Ar
gas. The crystal structure and composition of the Ga2O3 films were
characterized by x-ray diffraction (XRD). UV-vis diffuse reflectance
spectra were measured using UV-vis diffuse reflectance spectroscopy
(U-3900).
The growth temperature is known to play an important role in the
epitaxy of thin films.12,13 As a result, our investigations started with the
effect of growth temperature. First, the growth temperature in PECVD
is varied from 740  C to 880  C during the growth of the b-Ga2O3 epi-
layer. To be consistent, the Ar/O2 flow rate of 80/5 SCCM was used for
all the samples with a fixed RF power and distance of 120 W and 8 cm,
FIG. 1. Schematic diagram of the PECVD system.
Appl. Phys. Lett. 116, 072102 (2020); doi: 10.1063/1.5142196
Published under license by AIP Publishing
ARTICLE scitation.org/journal/apl
respectively. Our investigations showed that when the growth tempera-
ture is below 740  C, there are no peaks except for Al2O3-related diffrac-
tion peaks, indicating that the prepared b-Ga2O3 film is amorphous or
microcrystalline. As the growth temperatures are above 760  C, three
peaks located at 18.8 , 38.2 , and 58.9 , which correspond to
ð201Þ; ð402Þ; and ð603Þ of b-Ga2O3, were observed, indicating the
ð201Þ orientation in b-Ga2O3 films [Fig. 2(a)].12 These three b-Ga2O3
related diffraction peaks become stronger and sharper with the increase
in the growth temperature, which indicates the improvement of crystal-
line quality of epitaxial films. It is noted that some additional low inten-
sity peaks at 30.2 , 31.6 , and 35.2 appear as the temperature is above
860  C, which belong to other plane orientations of b-Ga2O3 [Fig. 2(b)].
The degradation of crystallinity is caused by destroying the arrangement
of atoms at excessive high growth temperature. To further characterize
the crystal quality of the b-Ga2O3 films grown at various temperatures,
XRD rocking curves of the ð201Þ plane of the b-Ga2O3 films were mea-
sured. The FWHM value increases after an initial decrease with the
increase in growth temperature and reaches the optimal value of 0.86
at 820  C [Fig. 2(c)]. As shown in Fig. 2(d), the growth rate increases
monotonically from 0.21 lm/h to 1.04 lm/h with the increase in the
growth temperature from 760  C to 880  C. The metallic Ga evapora-
tion rate increases as the temperature increases, and thus, the adatom
concentration in the substrate increases and the growth rate becomes
fast. For a comparison, the reported representative FWHM/growth rates
of heteroepitaxial b-Ga2O3 films grown on c-plane sapphire substrates
are listed in Table I. PECVD epitaxy films show a high growth rate of
0.58 lm/h and satisfactory crystallinity with a FWHM value of 0.86
at 820  C. As a comparison, the reported representative FWHM/growth
rates of heteroepitaxial b-Ga2O3 thin films grown on c-plane sapphire
substrates are 0.9 /0.09 lm/h (MBE),17 0.6 /0.24 lm/h (MOCVD),18
0.16 /0.22 lm/h (PLD),19 and 1.49 /1.71 lm/h (LPCVD).12 Recently,
Alema et al. reported high rate growth of epitaxial b-Ga2O3 thin films
on c-plane sapphire substrates using a close coupled showerhead
FIG. 2. XRD patterns (a) and the growth rates (d) of the b-Ga2O3 films deposited
on c-sapphire substrates at various temperatures. (b) The enlarged XRD patterns
of the b-Ga2O3 films deposited at 860  C and 880  C. (c) XRD rocking curve of the
ð201Þ plane of the b-Ga2O3 epilayer grown at 820  C.
116, 072102-2
 Applied Physics Letters
TABLE I. Comparison of the FWHM values and the growth rates of heteroepitaxial b-Ga2O3 thin films grown on c-plane sapphire substrates from this work and other previously
reported.
MOCVD MBE
Temperature 900  C 960  C
Growth rate 10 lm/h 0.09 lm/h
FWHM … 0.9
MOCVD reactor. The growth rates achieve 10 lm/h using TMGa at a
substrate temperature of 900  C.21 Zhao et al. reported heteroepitaxial
growth of b-Ga2O3 thin films on off-axis (0001) c-sapphire substrates by
LPCVD. The b-Ga2O3 film grown on 6 off-axis c-sapphire exhibits a
high growth rate (6 lm/h) with a FWHM of 0.47 .22 The b-Ga2O3
epitaxial film growth by the PECVD method exhibits an excellent com-
prehensive performance at low growth temperature. In addition, consid-
ering that all materials used in this technique are Ga metal and oxygen
and Ar gases (which are cheap, environmentally friendly, and easy to
acquire), PECVD could potentially be suitable for industrialized produc-
tion of the b-Ga2O3 epilayer.
The UV-vis absorption edge of the b-Ga2O3 epilayer appears at
280 nm and shifts to a longer wavelength as the temperature increases
to 860  C [Fig. 3(a)]. The bandgaps of b-Ga2O3 are estimated from the
curves of (ah)2 vs hv on the basis of the UV-vis absorbance spectra
[Fig. 3(b)]. The bandgap decreases first and then increases as the tem-
perature increases. The decrease in the bandgaps is caused by the ther-
mal expansion of the lattice, as well as the increase in atomic vibration
and electron-phonon interaction.3,14 Since b-Ga2O3 has an anisotropy
for the optical properties, the increase in bandgap energy at 880  C
may originate from the formation of b-Ga2O3, exhibiting different
plane orientations.
Second, the effects of Ar and O2 flow rates on the b-Ga2O3 epi-
layer were studied systematically. All the growth was completed using
the fixed temperature, RF power, and distance of 820  C, 120 W, and
8 cm, respectively. As the O2 flow rate increases from 0 to 5 SCCM,
the diffraction peaks of the b-Ga2O3 epilayer are stronger and sharper,
indicating the improvement of crystalline quality [Fig. 4(a)]. There
exist many intrinsic defects such as oxygen vacancies in the films,
resulting in the chemical composition of Ga2O3 being non-
stoichiometric. The increase in the O2 flow rate could reduce the oxy-
gen vacancies. According to nucleation theory, nucleation density can
be described by the following equation:15
FIG. 3. (a) UV-vis spectra of the b-Ga2O3 films grown at various temperatures; the
inset shows a partially enlarged view. (b) Bandgap of the b-Ga2O3 films as a func-
tion of growth temperature.
Appl. Phys. Lett. 116, 072102 (2020); doi: 10.1063/1.5142196
Published under license by AIP Publishing
ARTICLE scitation.org/journal/apl
PLD LPCVD HVPE Our work
800  C 900  C 1000  C 820  C
0.22 lm/h 6 lm/h 5.01 lm/h 0.58 lm/h
0.16 0.47 … 0.8
N ¼ Aexpð䉭G =RT Þ; (1)
where N is the nucleation density and 䉭G is the activation energy of

nucleation, which is composed of volume free energy 䉭GV and surface
free energy 䉭GS. For the chemical reaction of 4Ga þ 3O2 ¼ 2Ga2O3,
as䉭GV /-In P(O2), the free energy change per unit volume 䉭GV
decreases with the increasing concentration of oxygen.16 As the O2
flow rate increases from 5 to 40 SCCM, the diffraction peaks of the
b-Ga2O3 epilayer are weaker and wider, indicating the degradation of
crystalline quality. As the O2 flow rate continuously increases, the
excessively high nucleation rate results in the deposited particles being
unable to migrate to the appropriate lattice positions, and the films
grew and oriented in unsuitable directions, which caused random
growth and crystalline quality degradation. The growth rate of the film
increases first and then decreases as the O2 flow rate increases, which
reaches the maximum value of 0.58 lm/h with the O2 flow rate of
5 SCCM [Fig. 4(b)]. Under a higher O2 flow rate, Ga was rapidly oxi-
dized, and the evaporation of the Ga source has been suppressed.17
As the Ar flow rate increases, the diffraction peaks of the ð201Þ
plane family become sharper, indicating the improvement of crystal-
line quality [Fig. 4(c)]. Meanwhile, the growth rate increases linearly
from 0.28 lm/h to 0.61 lm/h with the increase in the Ar flow rate
from 30 to 100 SCCM [Fig. 4(d)]. With a higher Ar flow rate, the oxy-
gen molecules could undergo less collision with the gallium vapor,
FIG. 4. XRD patterns (a) and growth rates (b) of the b-Ga2O3 films deposited at
various oxygen flow rates. XRD patterns (c) and growth rates (d) of the b-Ga2O3
films deposited at various argon flow rates.
116, 072102-3
 Applied Physics Letters
leading to less consumption of oxygen species. Hence, the adatom
concentration in the substrate increases as the Ar flow rate increases,
which improves the growth rate of b-Ga2O3 epitaxial films.
Third, the effects of the distance between the substrate and the
Ga source (from 4 cm to 12 cm) on the b-Ga2O3 epilayer were per-
formed. The growth temperature was set to 820  C, the gas flow rate of
Ar/O2 was set to 80/5 SCCM, and the RF power was fixed at 120 W.
As shown in Figs. 5(a) and 5(b), the growth rate decreases with the
increase in the distance. For the PECVD setup, second order Fick’s
law was used and assuming that all the oxygen that reaches the sub-
strate surface, or the reactor wall is consumed or deposited, and the
radial concentration gradient at the center of the chamber is zero, the
growth rate as a function of x can be written as
2DMGa2 O3 C0 DxP22
RðxÞ ¼ e 4Vd ; (2)
dqMO2
where q is the volume mass density of b-Ga2O3, C0 is the density of
oxygen at the location of the Ga source, and M represents the molecu-
lar weight of the species. As shown in Fig. 5(b), the decrease in the
growth rate with the increase in the distance is consistent with Eq. (2).
Finally, the effect of RF power (0, 80, 120, 180, 240, and 280 W)
was studied. The growth temperature was set to 820  C, and the Ar/O2
flow rate was kept at 80/5 SCCM. The increase in RF power leads to
the increase in the ionization rate of O atoms, which will increase the
mobility of deposited atoms and improve the crystal quality of the
films [Fig. 5(c)]. However, the crystallinity of b-Ga2O3 films decreases
as the RF power sequentially increases to 280 W. (1) Insufficient time
for atoms to diffuse to their sites, and hence, the films grew and ori-
ented in unsuitable directions; (2) high-energy plasma will etch the
surface of the as-grown films. The growth rate of b-Ga2O3 epilayers
monotonously increases with the increase in RF power [Fig. 5(d)],
which can obtain >1 lm/h with a power of 200 W. For a typical
FIG. 5. XRD patterns (a) and growth rates (b) of the b-Ga2O3 films grown at
various distances between the Ga source and substrate. XRD patterns (c) and
growth rates (d) of the b-Ga2O3 films grown at various RF powers.
Appl. Phys. Lett. 116, 072102 (2020); doi: 10.1063/1.5142196
Published under license by AIP Publishing
ARTICLE scitation.org/journal/apl
FIG. 6. Mechanism for nucleation and growth of the b-Ga2O3 epilayer.
atomic diffusion process, the diffusion coefficient conforms to
Arrhenius’ law,18
 
Q
D ¼ D0 exp ; (3)
KT
where D0 is the diffusion constant, Q is the diffusion activation energy
of atoms, and T represents the temperature. Plasma treatment of the
gas mixture in the CVD process allows the reduction of activation
energy of adatoms and increase in the growth rate by a few orders of
magnitude compared to that in the thermal CVD process.19,20
According to our sample characterization and growth experi-
ments, a proposed model for the mechanism of nucleation and growth
of the Ga2O3 epitaxial film is shown in Fig. 6. This involves a number
of steps: (I) Ga vapor generated from the precursor material at high
temperature was transported to the substrate by the carrier gas and
was adsorbed at suitable substrate surface sites. (II) Stable O2 was
excited into the O plasma by the high RF energy, which has a high
Gibbs free energy. To reduce the Gibbs free energy, the active O
plasma begins to deposit on the surface of the substrate and migrate to
nearby stable atoms. As the atoms continue to migrate and deposit,
the crystal nuclei of Ga2O3 are formed. (III) With more Ga and O
atomic absorbed in the substrate, nucleation two-dimensional Ga2O3
islands are formed. Finally, the Ga2O3 films are formed upon the
nucleated Ga2O3 islands. Also, the close lattice match and crystal sym-
metry between b-Ga2O3 and sapphire promoted the uniform thin film
growth.
The b-Ga2O3 epitaxial film grown on the c-plane sapphire sub-
strates by the PECVD method possesses a high growth rate of
0.58 lm/h and a single ð201Þ plane orientation with a FWHM value
of 0.86 at 820  C. A proposed model for the mechanism of nucleation
and growth of the b-Ga2O3 epilayer is established to help us better
understand the precursor transport and gas phase reaction process. In
addition, considering that all materials used in this technique are Ga
metal and oxygen and Ar gases (which are cheap, environmentally
friendly, and easy to acquire), PECVD could potentially be suitable for
industrialized production of the b-Ga2O3 epilayer.
This work was supported by the National Natural Science
Foundation of China (Nos. 61704153, 61764001, and 61774019),
Zhejiang Public Service Technology Research Program/Analytical
116, 072102-4
 Applied Physics Letters ARTICLE scitation.org/journal/apl

8
Test (No. LGC19F040001), Natural Science Foundation of Zhejiang D. Y. Guo, X. L. Zhao, Y. S. Zhi, W. Cui, Y. Q. Huang, Y. H. An, P. G. Li, Z. P.
Province (No. LY20F040005), Guangxi Science and Technology Wu, and W. H. Tang, Mater. Lett. 164, 364–367 (2016).
9
C. R. He, D. Y. Guo, K. Chen, S. L. Wang, J. Q. Shen, N. Zhao, A. P. Liu, Y. Y.
Base and Talent Special Project (No. AD18281084), Visiting
Zheng, P. G. Li, Z. P. Wu, C. R. Li, F. M. Wu, and W. H. Tang, ACS Appl.
Scholar Foundation of State Key Lab of Silicon Materials (No. Nano Mater. 2(7), 4095–4103 (2019).
SKL2019-08), Open Fund of Key Laboratory of Cognitive Radio 10
K. Chen, C. R. He, D. Y. Guo, S. L. Wang, Z. W. Chen, J. Q. Shen, and P. G. Li,
and Information Processing Ministry of Education (Guilin J. Alloys Compd. 755, 199–205 (2018).
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Chem. Phys. 133, 700–705 (2012).
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Appl. Phys. Lett. 116, 072102 (2020); doi: 10.1063/1.5142196 116, 072102-5
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