Received: 30 August 2022 Revised: 25 October 2022 Accepted: 29 November 2022

DOI: 10.1002/bio.4510

RESEARCH ARTICLE

Rapid synthesis of BaMoO4:Eu3+ red phosphors using

microwave irradiation

Zhao Li | Ju-long Cheng | Ya-nan Wang | Kun-yao Wu | Jing Cao

Xi'an Aeronautical Institute, School of

Materials Engineering, Xi'an, China Abstract
This study synthesized BaMoO4:Eu3+ red phosphors using the microwave method.
Correspondence
Zhao Li, Xi'an Aeronautical Institute, School of In addition, the phase composition, morphology, and luminescence properties of the
Materials Engineering, Xi'an 710077, China.
red phosphors were characterized using X-ray diffraction, field-scanning electron
Email: [email protected]
microscopy, and photoluminescence spectroscopy. The results revealed that doping
Funding information
red phosphors with different concentrations of Eu3+ does not change the crystal
Xi'an Science and Technology Committee
Program, Grant/Award Number: GXYD9.2; structure of the matrix material. The BaMoO4:Eu3+ phosphors exhibited micron-scale
Shaanxi Educational Committee, Grant/Award
irregular polyhedra, which could be excited by ultraviolet light with a wavelength of
Number: 17JK0395
395 nm to induce red-light emission. The optimal dosage of Eu3+ was 0.08, and the
chromaticity coordinates of BaMoO4:0.08Eu3+ phosphors were (0.5869, 0.3099).
White light-emitting diode (w-LED) devices manufactured by using a combination of
BaMoO4:0.08Eu3+ phosphor and commercially available phosphors exhibited good
white-light emission under the excitation of an ultraviolet chip. The
3+
BaMoO4:0.08Eu red phosphors that rapidly synthesized under the microwave field
are expected to be used in w-LED devices.

KEYWORDS
BaMoO4:Eu3+, device, microwave irradiation, white light-emitting diodes

1 | I N T RO DU CT I O N Eu3+-activated tellurite samples were synthesized. Glass ceramic

containing Eu2Te6O15 microcrystals was obtained as a function of
As fourth-generation lighting sources, white light-emitting diodes (w- crystallization time from 0 to 4 h at 435
C. Our research group has
LEDs) exhibit advantages such as energy conservation, environmental synthesized the ScVO4:Eu3+ red phosphor [12]. However, the synthe-
protection, high reliability, and durability. w-LEDs can be widely used sis method is time consuming. The microwave method has been
in various fields such as display techniques, lighting, sensing, and plant developed as a new tool in phosphors. During the heating process,
growth [1–4]. Currently, w-LEDs are produced mainly by the combi- the electromagnetic wave penetrates the materials and heats them
nation of a blue LED chip and a YAG:Ce3+ yellow phosphor. The main due to the interaction between the polarized molecules (or ions) and
limitation of this combination is the low color rendering caused by the the electromagnetic field, finally resulting in volumetric heating. The
lack of the red-light component in the YAG:Ce3+ yellow phosphor. volumetric heating ability of microwaves enables a more rapid and
Among existing phosphors with a high optical conversion efficiency uniform heating, decreases the processing time, and finally enhances
and excellent thermal stability, a few red phosphors can be effectively the material properties [13]. In this study, microwave irradiation was
excited using near-ultraviolet (n-UV) light [5–8]. Eu3+ can be absorbed employed to synthesize BaMoO4 phosphor doped with Eu3+
in the n-UV and blue regions [9, 10]; therefore, Eu3+-doped lumines- rare-earth metal ions, and its phase structure, apparent morphology,
cent materials has been widely studied. Desirena et al. [11] designed a and luminescence properties were investigated. The innovation point
phosphor for n-UV-based w-LEDs with a low correlated color of this study was the preparation of irregular polyhedra BaMoO4
temperature and a high color rendering index (CRI); a series of highly powder that could be excited by ultraviolet light and blue light using

1414 © 2023 John Wiley & Sons Ltd. wileyonlinelibrary.com/journal/bio Luminescence. 2023;38:1414–1421.
 15227243, 2023, 8, Downloaded from https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/10.1002/bio.4510 by UNIVERSIDADE ESTADUAL DE MATO GROSSO DO SUL, Wiley Online Library on [26/03/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
LI ET AL. 1415

microwave irradiation. The main excitation peak corresponding to

BaMoO4:Eu3+ phosphor was observed at 395 and 464 nm, thus mak-
ing it the most suitable phosphor to be used as the red-light compen-
sation powder of green or yellow phosphors excited by ultraviolet
light or blue light.

2 | PREPARATION AND
CHARACTERIZATION OF MATERIALS

2.1 | Preparation of BaMoO4:Eu3+ red phosphors

Pure BaCO3, MoO3, and Eu2O3 raw materials were accurately

weighed according to the stoichiometric ratio and transferred to an
agate mortar. An appropriate quantity of absolute ethanol was added
F I G U R E 1 XRD (X-ray diffraction) patterns of BaMoO4:Eu3+ red
into the agate mortar, and the raw materials were ground for 40 min phosphors with different Mn4+ doping concentrations.
until absolute ethanol was completely volatilized. The evenly mixed
powder was transferred into a 5-ml corundum crucible, and the pow-
der in the corundum crucible was subsequently transferred into a
15-ml crucible loaded with granular activated carbon. The 15-ml cruci-
ble was placed on a glass turntable in a microwave oven, and the
mixed powder was pyrolyzed at 560 W for 30 min, producing
BaMoO4:Eu3+ phosphors.

2.2 | Characterization

The crystal structure of BaMoO4:Eu3+ red phosphors was character-

ized using an X-ray diffractometer (Rigaku Ultima IV, Japan). The mor-
phological characteristics of the sample were studied using a field-
emission scanning electron microscope (Zeiss Sigma 300, Bruker,
Germany). The excitation and emission spectra of the phosphor were
measured using a fluorescence spectrophotometer (Hitachi F7000).
The chromaticity coordinates and CRI of the assembled LED device
were measured using an LED device testing system (Hongpu
HP9000). All the tests were performed at room temperature. FIGURE 2 XRD (X-ray diffraction) refinement of BaMoO4:Eu3+
phosphor.

3 | RESULTS AND DISCUSSION into the BaMoO4 lattice, albeit with no change in the crystal structure
of the base material.
3.1 | Phase structure analysis To further obtain crystal structure information on the phosphors,
General Structure Analysis System software was employed for Riet-
Figure 1 shows the X-ray diffraction (XRD) patterns of BaMoO4:Eu3+ veld structure refinement on the XRD data of BaMoO4:0.08Eu3+
phosphor samples synthesized using the microwave method. The dif- phosphor. Figures 2 and 3 show the refined XRD pattern and the cor-
fraction peaks of BaMoO4:Eu3+ phosphors with different Eu3+ dos- responding crystal cell structure, respectively. The refined XRD pat-
ages synthesized using microwave irradiation are consistent with tern of the BaMoO4:0.08Eu3+ phosphor is consistent with its XRD
those of the standard card (PDF#29-0193), among which the diffrac- pattern (Figure 2). The parameters of the Rietveld structure refine-
tion peak corresponding to the (112) crystal plane exhibits the highest ment are as follows: the full spectrum factor Rp = 7.15%, the
intensity. The synthesized sample belongs to the scheelite structure weighted full spectrum factor Rwp = 9.29%, and the fitting degree is
of a body-centered tetragonal crystal system. Other miscellaneous x2 = 1.197. The refinement results are credible. The crystal structure
peaks are not observed in the XRD patterns, and impure phases are parameters of BaMoO4 are a = 5.58 Å, c = 12.82 Å, and
not produced in the samples, indicating the successful doping of Eu3+ V = 399.23 Å3. Table 1 summarizes the lattice constants and atomic
 15227243, 2023, 8, Downloaded from https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/10.1002/bio.4510 by UNIVERSIDADE ESTADUAL DE MATO GROSSO DO SUL, Wiley Online Library on [26/03/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
1416 LI ET AL.

FIGURE 3 Crystal structure of BaMoO4:Eu3+ phosphor.

T A B L E 1 Lattice constant and atomic

BaMoO4 Atom Oxidation state Occupancy x y z
position of BaMoO4 crystal.
a = b = 5.5840 Å Ba +2 1 0 0.2500 0.1250
c = 12.8262 Å Mo +6 1 0 0.6250 0.6250
α = β = γ = 90
O 2 1 0.6074 0.2033 0.2033

positions of the Eu3+-doped BaMoO4 crystal after XRD refinement.

The crystal parameters of BaMoO4:0.08Eu3+ phosphor are
a = 5.58 Å, c = 12.83 Å, and V = 399.93 Å3. By comparison, the
BaMoO4 crystal expands slightly after Eu3+ doping. The ionic radius
of Eu3+ is 0.95 Å, whereas that of Mo6+ is 0.56 Å, which is consider-
ably less than that of Eu3+. Moreover, Mo6+ and O2 can form anion
compounds and cannot be separated easily. Compared to Ba2+ with
an ionic radius of 1.35 Å, Eu3+ exhibits an effective lower radius. Con-
sequently, Eu3+ can be doped into the BaMoO4 crystal to form an
interstitial solid solution in the lattice interspace, leading to the expan-
sion of the BaMoO4 lattice and enlarging the BaMoO4 crystal.

3.2 | Photoluminescence spectrum analysis

Figure 4 shows the excitation spectra of BaMoO4:Eu3+ phosphor

samples synthesized using microwave irradiation. A strong broad band FIGURE 4 Excitation spectrum of BaMoO4:Eu3+ phosphor.
and several sharp peaks can be observed in the spectrum. The broad
band centered at 297 nm is attributed to the well-known O2 ! Eu3+-
charge transfer absorption [14, 15]. A series of excitation peaks after
350 nm of the samples exhibit two main excitation peaks at 395 and to the 7F0 ! 5D2 transition of Eu3+ [16]. The wavelength of the exci-
464 nm, respectively. The absorption peak at 395 nm is attributed to tation light corresponding to the strongest excitation peak is 395 nm,
the 7F0 ! 5L6 transition of Eu3+, whereas that at 464 nm is attributed which lies in the ultraviolet-light range. Therefore, the BaMoO4:Eu3+
 15227243, 2023, 8, Downloaded from https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/10.1002/bio.4510 by UNIVERSIDADE ESTADUAL DE MATO GROSSO DO SUL, Wiley Online Library on [26/03/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
LI ET AL. 1417

phosphor samples synthesized using the microwave method can be

effectively excited by ultraviolet light and blue light.
Figure 5 shows the emission spectra of BaMoO4:Eu3+ phosphors
at different Eu3+ doping concentrations. The strongest emission peak
of BaMoO4:Eu3+ phosphor is located at 618 nm, corresponding to
the characteristic emission peak of the 5
D0 ! 7F2 electric dipole
3+
transition of Eu [17]. The weaker peaks located at 596 and 701 nm
of Eu3+doped BaMoO4 phosphor correspond to the 5D0 ! 7F1 and
5
D0 ! 7F4 transitions of Eu3+, respectively [18]. Different doping
concentrations of Eu3+ do not change the position of the characteris-
tic emission peak but only the luminescence intensity of the phos-
phor. With the increase in the Eu3+ dosage to 8%, the luminescence
intensity of the sample reaches the peak value. At a Eu3+ dosage of
less than 8%, a few luminescent centers are present, with a long dis-
tance between them; therefore, there is almost no interaction. Mean-
while, at an Eu3+ dosage of greater than 8%, excess activator ions
lead to the decrease in the average distance between the lumines-
cence centers in the lattice, and strong interactions between lumines-
cence centers exist. Thus, the probability of energy transfer is greater F I G U R E 6 Emission spectrum of BaMoO4:Eu3+ phosphor at
than that of energy conversion into irradiation transition. Therefore, different charge compensation.

the probability of concentration quenching when the excited photons

encounter the quenching centers increases, leading to the decrease in
the luminescence intensity. Compared to Na+ charge compensation, after Li+ charge compensa-
+ +
The effects of charge compensation of Li and Na on the emis- tion, the luminescence intensities of the samples can be improved
sion intensity of BaMoO4:Eu3+ phosphor under excitation light at a more significantly under the same dosage of charge compensators,
wavelength of 395 nm were investigated. Figure 6 shows the emis- because as charge compensating agents, Li+ and Na+ can balance the
sion spectra. The addition of the charge compensator changes the charge imbalance caused by the equivalent substitution of Eu3+ for
3+
luminescence intensities of BaMoO4:Eu phosphors and not their Ba2+, which can improve the luminescence intensity of the phosphor
emission peak positions. The luminescence intensity of the samples is samples after charge compensation. The rare-earth Eu3+ ions exhibit
enhanced under the action of the two charge compensators. a valence state of +3; however, Ba2+ ions always exhibit a valence
state of +2. When the Ba2+ ions with +2 valence state are
substituted by Eu3+ ions, the charge differences produce vacancies of
positive charge. Conversely, when the alkaline-earth metal ions are
substituted by earth ions with +1 valence state, the charge differ-
ences produce vacancies of negative charge. Thus, the charge imbal-
ance and lattice stress can be reduced. Therefore, the lattice structure
is more intact, which can effectively reduce nonradiative transition
and change the luminescent properties. In addition, when charge com-
pensators are doped into the matrix lattice, Li+ with a smaller radius
(RLi+ = 0.076 nm) causes a slight lattice distortion than Na+ with a
larger radius (RNa+ = 0.102 nm). Li+ doping reduces the probability of
crystal defects caused by Eu3+ (REu3+ = 0.0947 nm). Therefore, the
luminescence intensity of the samples after Li+ charge compensation
is higher.

3.3 | Morphology and energy-dispersive spectrum

analysis

Figure 7 shows the field-emission scanning electron microscopic

images of BaMoO4:0.08Eu3+ phosphor samples under different mag-
F I G U R E 5 Emission spectrum of BaMoO4:Eu3+ phosphor at nifications. The BaMoO4:0.08Eu3+ phosphor exhibits irregular polyhe-
different Eu3+ doping concentrations. dra, with particle sizes in the range of 2–3 μm. The size and
 15227243, 2023, 8, Downloaded from https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/10.1002/bio.4510 by UNIVERSIDADE ESTADUAL DE MATO GROSSO DO SUL, Wiley Online Library on [26/03/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
1418 LI ET AL.

F I G U R E 7 Field-scanning electron
microscopic images of BaMoO4:0.08Eu3+ (a)
2000, (b) 5000, (c) 10000, and (d) 20000.

F I G U R E 8 Scanning point determination of BaMoO4:Eu3+ phosphor. (a) the element composition after EDS point scanning at one arbitrary
points and (b) the element composition after EDS point scanning at another arbitrary points.

morphology of the particles and the dispersibility of the phosphors BaMoO4:0.08Eu3+ phosphor sample. According to the scanning
affect their luminous flux, optical decay, and encapsulation and coat- results, only Ba, Mo, O, and Eu are present at the two points. Further-
ing performance. An extremely large particle size can lead to the more, the distribution of all elements in the sample can be obtained
uneven coating of phosphors, whereas an extremely small particle size by EDS mapping analysis of the BaMoO4:0.08Eu3+ phosphor sample.
may reduce the absorption for n-UV irradiation and enhance n-UV Figure 9 shows the mapping results. According to the mapping results,
irradiation, thus reducing the luminescence efficiency [19, 20]. the sample contains O, Mo, Ba, and Eu, without other impurity ele-
Figure 8 shows the element composition after energy-dispersive ments. Combined with XRD results, Eu3+ is confirmed to be success-
spectrum (EDS) point scanning at two arbitrary points of the fully doped into the matrix lattice of BaMoO4:Eu3+ red phosphor.
 15227243, 2023, 8, Downloaded from https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/10.1002/bio.4510 by UNIVERSIDADE ESTADUAL DE MATO GROSSO DO SUL, Wiley Online Library on [26/03/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
LI ET AL. 1419

FIGURE 9 Mapping images of BaMoO4:Eu3+ phosphor. (a) Eu, (b) O, (c) Mo, and (d) Ba.

3.4 | Color coordinate and luminescence

mechanism analysis

Figure 10 shows the color coordinates of BaMoO4:0.08Eu3+

phosphor calculated from the emission spectrum data of the
BaMoO4:0.08Eu3+ phosphor sample. The chromaticity coordinates
of the BaMoO4:0.08Eu3+ phosphor sample are (0.5869, 0.3099),
corresponding to the red-light region in the chromaticity map; this
result indicates that BaMoO4:Eu3+ phosphors can emit red light.
Figure 11 shows the schematic of the luminescence mechanism of
the BaMoO4:Eu3+ phosphor. As the matrix of the BaMoO4:Eu3+
phosphor, BaMoO4 exhibits a scheelite structure of the tetragonal
crystal system. Due to the special properties of the [MoO4]2
group, the charge migration of electrons from O2 to Mo6+ occurs;
therefore, the BaMoO4 matrix can well absorb ultraviolet excitation
energy. Moreover, the absorbed ultraviolet excitation energy can
be transferred to the doped Eu3+; therefore, Eu3+ exhibits good
luminescence. For Eu3+, the f–f electron transition can induce its
irradiation fluorescence. The transfer of energy between the
[MoO4]2 group and Eu3+ in the phosphor during the luminescence
process is observed (Figure 11). Under excitation at a wavelength of
FIGURE 10 Color coordinates of BaMoO4:0.08Eu 3+
phosphor. 395 nm, the electrons in the [MoO4]2 group are transferred from

FIGURE 11 Luminescence mechanism diagram.

 15227243, 2023, 8, Downloaded from https://analyticalsciencejournals.onlinelibrary.wiley.com/doi/10.1002/bio.4510 by UNIVERSIDADE ESTADUAL DE MATO GROSSO DO SUL, Wiley Online Library on [26/03/2025]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
1420 LI ET AL.

the ground state to the excited state. The excited electrons in the chromaticity diagram. Therefore, the BaMoO4:Eu3+ red phosphor
5
excited state are transferred to the D0 energy level of Eu3+, synthesized under the microwave-field condition is expected to be
3+
and then Eu radiates and emits light. The emission spectrum of applied to w-LED devices.
Eu3+ is composed of the characteristic emissions of D0 ! 7FJ
5

(J = 1, 2, 3, and 4), and the electric dipole transition (5D0 ! 7F2)

at 618 nm is the strongest, manifesting as the red-light emission 4 | CONC LU SIONS
3+
of Eu [21].
BaMoO4:xEu3+ (x = 2%, 4%, 6%, 8%, and 10%) red phosphors were
synthesized using the microwave method. The diffraction peaks of
3.5 | Analysis of the w-LED device manufactured BaMoO4:Eu3+ phosphors were in good agreement with the standard
using BaMoO4:Eu3+ phosphor card data of BaMoO4. The doping of Eu3+ did not change the
crystal structure of the matrix material, and the prepared samples
The BaMoO4:Eu3+ phosphor synthesized rapidly under the exhibited a pure tetragonal scheelite structure. The BaMoO4:Eu3+
microwave-field condition was packaged. According to a phosphor to phosphor sample was effectively excited by ultraviolet light at a
glue mass ratio of 1:0.8, the organic silica gel was mixed with red, wavelength of 395 nm, and it exhibited a strong red-light emission
green, and blue phosphors (the mass ratio of red, green, and blue at 618 nm. At a Eu3+ dosage of 8%, the maximum emission inten-
phosphors was 5:1:2). The red phosphor was the synthesized sity was attained, and the luminescence intensity significantly
BaMoO4:Eu3+ red phosphor sample, and the green and blue phos- improved after Li+ charge compensation. The chromaticity coordi-
2+
phors were commercial (Ba, Sr)2SiO4:Eu green phosphor and com- nates of the emitted light were (0.5869, 0.3099), corresponding to
mercial BaMgAl10O17:Eu2+ blue phosphor, respectively. The mixed the red-light range of the chromaticity map. The products exhibited
phosphors and organic silica gel were assembled using a 395 n-UV micron-scale irregular polyhedra, and the chromaticity coordinates
chip to obtain a w-LED device. Figure 12 shows the spectrum diagram of the LED device packaged using the mixture of the synthesized
of the assembled w-LED device, and the insets in Figure 12 show the BaMoO4:Eu3+ phosphor and commercial phosphors were (0.2896,
image of the assembled w-LED device and the image after the device 0.2799), corresponding to the white-light region. The BaMoO4:Eu3+
is lit. The chromaticity coordinates of the w-LED device packaged red phosphor synthesized rapidly using microwave irradiation is
using our synthesized BaMoO4:Eu3+ red phosphor sample are expected to be used in w-LEDs.
(0.2896, 0.2799), corresponding to the white-light region in the
ACKNOWLEDG MENTS
This work was financially supported by Xi'an Science and Technology
Committee Program (No. GXYD9.2) and Shaanxi Educational Commit-
tee (No. 17JK0395).

DATA AVAILABILITY STAT EMEN T

All data used during the study are available from the corresponding
author by request.

OR CID
Zhao Li https://orcid.org/0000-0002-1463-873X

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