Ceramics International xxx (xxxx) xxx

Contents lists available at ScienceDirect

Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Highly efficient and thermally stable MnII-based phosphor-in-glass towards

warm WLED
Tianpeng Liu a, Xiaoshuang Li a, *, Kang Zhang a, Shuwei Deng a, Zhiyu Hu a, Hongxiang An a,
Bo Wang a, Youchao Kong b, **
a
School of Applied Physics and Materials, Wuyi University, Jiangmen, Guangdong, 529020, PR China
b
Department of Physics and Electronic Engineering, Yancheng Teachers University, Yancheng, 224002, China

A R T I C L E I N F O A B S T R A C T

Keywords: Aluminate with the magnetoplumbite-type (LaZnAl11O19) represents a big family technology important com­
Phosphor pound. Crystallographic sites for transition metal and rare earth ion in the magnetoplumbite structure have
Luminescence always been a hot topic. Here, manganese-based magnetoplumbite-type La(Zn,Mn)Al11O19 phosphors were
Glass-ceramic
successfully synthesized via the traditional solid-state reaction and all the samples crystallized into the hexagonal
LED
structure. A narrow green emission band at approximately 518 nm with quantum efficiency (~unit one) is
demonstrated in LaZnAl11O19 host with Mn2+ doping equal 0.3. Temperature dependent photo-luminescence
indicate that LaZn0.7Mn0.3Al11O19 sample keep excellent thermal stability. Meanwhile, the thermal ionization
process was elaborated in detail. At last, a high-power w-LED with a high color rendering index and low asso­
ciated color temperature is produced by inserting the microcrystals into the glass host using a “phosphor-in-glass
(PiG)” technique.

1. Introduction
The construction of display devices with a broad color gamut (CG)
and high resolution is now feasible thanks to the new backlighting field
of liquid displays (LCD) [1–5]. Phosphor-converted white light-emitting
diodes (PC-WLEDs) have made inroads into high-definition display
systems, often using a mix of blue chip and narrow-emission phosphors
[6–9]. To date, as the optimum green phosphor, β-SiAlON:Eu2+, has
been extensively employed in the commercial LCD backlights [10]. The
large full-width at half-maximum (FWHM~55 nm) and the harsh
preparation condition result in limiting for application. Other rare earth
Eu2+ activated nitride, such as Ba [Li2(Al2Si2)N6], also face the problem
of high-costs [11]. Eu2+ doped SrGa2S4 presents a relatively smaller
FWHM, the low chemical stability is an unavoidable problem [12]. More
recently, Xia et al. discovered series of narrow-band green-emitting
phosphors, exhibiting good potential for LCD backlights application
[13]. In contrast, semiconductor perovskite CsPbBr3 quantum dots
owing a super-narrow emission peak (FWHM~20 nm) show good po­
tential for wide CG LCD applications [14–19]. Presently, the stability of
QDs has been greatly improved by the efforts of researchers, CsPbBr3
QDs show great commercial prospects. However, the toxicity and ther­
mal quenching property of QDs inhibit its further application [20].
Consequently, discovering higher physicochemical stability and nar­
rower green emitters suitable for CG of the pc-backlighting devices are
still continuously pursued by material scientists.
In comparing with the rare earth Eu2+-activated green phosphor or
perovskite CsPbBr3 QDs, transition metal Mn2+ doped one has attracted
increasing attention owing to the good luminescence properties [21].
Owing to the d-d transition, high luminescence and color purity green
emission can be obtained when the Mn2+ ions are surrounded by four
ligands. For example, Mn2+ activated Zn2SiO4 and BaAl12O19 have been
extensively used in the field of plasma display panels (PDP) and
field-emission displays (FED) [22,23]. Moreover, the non-rare-earth
Mn2+ doped narrow green emission phosphors have gained increased
attention in application of LCD backlights recently. Li et al. developed a
high luminescent efficiency green phosphor, BaZnAl10O17:Mn2+, and
the CG value reaches as wide as 110% National Television System
Committee (NTSC) [24]. Zhu et al. reported a high color purity
Mn2+-activated Sr2MgAl22O36 phosphor and the fabricated WLED shows
a NTSC value of 127% [25]. Song et al. discovery that WLED device

* Corresponding author.
** Corresponding author.
E-mail addresses: lixiaoshuang12@mails.ucas.ac.cn (X. Li), yb87816@connect.um.edu.mo (Y. Kong).

https://doi.org/10.1016/j.ceramint.2022.10.203
Received 3 August 2022; Received in revised form 13 October 2022; Accepted 15 October 2022
Available online 20 October 2022
0272-8842/© 2022 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Please cite this article as: Tianpeng Liu, Ceramics International, https://doi.org/10.1016/j.ceramint.2022.10.203
T. Liu et al.
Fig. 1. (a) Schematic representation of LaZnAl11O19 structures. (b) Band
structure of LaZnAl11O19 unit cell with the PBE method.
based on MgAl2O4:Mn2+ green emitting phosphor and K2SiF6:Mn4+ red
phosphor exhibits a NTSC of 116% [21]. High-power LEDs used in
practical field, combination of phosphors and commercial blue LED
chip, are the mainstream technology of the further general style. How­
ever, a high junction temperature would inevitably accelerate the aging
of organic resin and degrade luminous efficacy when a high input cur­
rent working [26–29]. Phosphor-in-glass (PiG) is strongly expected to be
a good solution to overcome this bottleneck [30–32].
In this work, a Mn2+ doped narrow green emitting phosphor LaZ­
nAl11O19:Mn2+ with excellent thermal stability has been successfully
preparation. By conducting the XRD and TEM method, the phase purity
was verified. The photoluminescence (PL) peak intensity reaches its
maximum at Mn = 0.3 mol substituting for Zn sites. Phosphors doped
with high concentration of Mn2+ can be expected to have high absorp­
tion for the excitation light, and consequently, high PL output. Hence,
under 450 nm excitation, the QE of optimal doping sample can reach
near-unity. The temperature dependent luminescence properties have
been carefully investigated. To overcome the adverse effect of applying
organic material as the encapsulant in high-power WLED, we adopted
phosphor-in-glass (PiG) technique to fabricate novel green-emitting
glass. Furthermore, the green luminescent glass and the KSF:Mn4+
fluorescence film were chosen as green and red light component,
respectively, the LED device with a high color gamut of 114% NTSC vale
has been realized, showing that it has potential application in LCD
backlights.
Fig. 2. (a) (c) TEM and HRTEM images of LaZn0.7Al11O19:0.3Mn2+ single particle. (b) Selected area electron diffraction pattern. (dh) STEM and component maps of
LaZn0.7Al11O19:0.3Mn2+ single particle.
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2. Result and discussion
2.1. Phase and structure
As a representative compound of magnetoplumbite-type, the crystal
structure of LaZnAl11O19 consists LaO12 and AlOn/(Zn,Al)Om polyhedral
(where n = 5, 6 and m = 4) [33]. Part of Al3+ and Zn2+ ions occupy five
distinct crystallographic sites in the structure. Trivalent La3+ ions locate
at the mirror planes from the centers, which are well separated by spinel
blocks formed by corners sharing (Zn,Al)O4 tetrahedra and AlO6 octa­
hedra on each side of the mirror planes. Such a unique structure is
beneficial for isolating luminescent centers from local perturbations in
the c direction, thereby, hopefully obtaining a high efficiency quantum.
Fig. S1(a) shows the XRD patterns of LaZn1-xAl11O19:xMn2+ and re­
ported for the magnetoplumbite structure. The XRD Rietveld re­
finements result at x = 0.3 is shown in Fig. S1(b). The final reliability
factors Rwp, Rp and χ 2 are listed in Table S1, which proves the reliability
of the fitting.
The crystal structure, as a host material, owing a wide bandgap
(>3.3 eV) is beneficial to accommodate the electronic states of the
luminescent center. Meanwhile, the wide bandgap could increase the
thermal stability via inhibiting the photoionization process. Fig. 1(b)
displays the calculated band structure of the optimized LaZnAl11O19
structure. The LaZnAl11O19 revealed a direct bandgap of 3.72 eV, which
was close to the experimental one of 3.93 eV in Fig. S2(a). Despite it, the
bandgap was wide enough to accommodate the d-d transition of a Mn2+
ion. The density of states (DOS) of LaZnAl11O19 were presented in Fig. S2
(b). The conduction band was clearly shown to be made up of 3p states
of O and a little quantity of 3 d states of Zn, whereas the valence band
was constituted of 2p states of Al and 5 d states of La, as well as a minor
amount of 2p states of Zn.
To further verify the phase purity, HRTEM/SAED images were used
and the obtained results are display in Fig. 2(a)-(c). The distance be­
tween adjacent crystal fringes is measured in crystal planes (1 0 7) and
(1 1 2), and the d-spacing values are 0.2636 and 0.2708 nm, respec­
tively. The crystal planes angle is 80◦ between (1 0 7) and (1 1 2) planes.
Fig. 2(d) reveals the irregular morphology of LaZn0.7Al11O19:0.3Mn2+
with particles agglomeration, the size of which is generally < 5 μm. As
shown in Fig. 1(e–h), one LaZn0.7Al11O19:0.3Mn2+ particle is selected
for the energy dispersive X-ray spectroscopy (EDS) mapping images,
confirming that the elements La, Zn, Al, O and Mn are homogeneously
distributed in the region examined.
In order to assess the manganese (IV) center obtained in the
T. Liu et al.
Fig. 3. (a) (b) XPS and EPR spectrum of LaZn0.7Al11O19:0.3Mn2+ sample.
phosphor, the XPS and EPR were used to detect the valence of Mn in the
LaZnAl11O19 specimen, and the spectra are shown in Fig. 3(a)-(b). The
high-resolution XPS peaks of the as-synthesized sample could be
assigned to the Mn-2p and close to the reference standard of MnCO3
[34]. Then, the cryogenic EPR was measured to illustrate the magnetic
coupling behavior of the sample. As shown in Fig. 3(b), one broad peak
instead of six fine structures was observed, attributed to the high Mn
concentration. The cathodoluminescence (CL) spectrum of LaZ­
n0.7Al11O19:0.3Mn2+ was obtained (Fig. S3), which have an emission
peak at 518 nm and an FWHM of 29 nm, similar to the photo­
luminescence (PL) spectrum in Fig. S4(b).
2.2. Luminescent properties
The diffuse reflection (DR) spectra of LaZnAl11O19:xMn2+ in Fig. S4
(a) show a typical d-d transition of the Mn2+ ion in d5 configuration with
a tetrahedral coordination geometry. The intensity of the photo­
luminescence at emission wavelengths (λem) as a function of the exci­
tation wavelengths (λex) were measured at room temperature. The
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Fig. 4. (a) Photoluminescence (PL) contour plot for excitation and emission of
LaZn0.7Al11O19:0.3Mn2+. (b) Luminescence decay curves of LaZ­
n0.7Al11O19:0.3Mn2+ sample.
results for the as-prepared LaZn0.7Al11O19:0.3Mn2+ was plotted in Fig. 4
(a), in which two broad excitation bands exist in the fluorescence
spectra. In addition, the CIE (x, y) parameters were nearly unchanged
under various photon irradiations, which indicates that the as-
synthesized samples have good color stability. The optimal excitation
position was found at 450 nm and originates from Mn2+:6A1→4T (4G)
[35,36]. Two excitation positions of Mn2+ ion are in the range of
330–390 nm and 410–470 nm when monitored at 517 nm, corre­
sponding to the Mn2+ excitation transitions of 6A1→4E (4G), 4T2 and
6
A1→4T (4G), respectively, and the strongest absorption zone matched
well with the InGaN chip [21,25]. As shown in Fig. S4(b), the emission
peak of the LaZn0.7Al11O19:0.3Mn2+ has a narrower full width at
half-maximum (fwhm, 28 nm) compared to β-SiAlON (fwhm, 52 nm),
which means better color purity (~76.8%). Under 450 nm excitation,
the IQE and EQE of LaZn0.7Al11O19:0.3Mn2+ could nearly reach to be
unity and 31.7%, respectively. The fluorescence decay curves of LaZ­
n0.7Al11O19:0.3Mn2+ phosphors monitored at 517 nm with the excita­
tion of 450 nm were measured (Fig. 4(b)). The predicted lifetimes of
Mn2+ ions are in the microsecond range, indicating that intra-d-shell
transitions in Mn2+ ions are banned.
2.3. Temperature-dependent photoluminescence and the mechanism of
the thermal quenching
The internal temperature of the chip may increase to more than 450
K when the high-power LED chip works. So, thermal stability will
significantly affect output lifetimes and the practical application of
green phosphor [37]. As shown in Fig. 5(a), the emission peaks exhibited
T. Liu et al. Ceramics International xxx (xxxx) xxx

Fig. 5. (a) Temperature-dependent emission spectra and the corresponding

optical microscopy. (b) (c) Temperature-dependent integrated emission in­
tensity and corresponding emission lifetime of LaZn0.7Al11O19:0.3Mn2+.

a slightly decrease with integrated PL intensities remain 92.4% at 470 K

of the initial intensity measured at 300 K. The activation energy Ea was
calculated to be 0.22 eV, according to the Arrhenius function [38].
Meanwhile, the shape of the emission spectra almost remained un­
changed when temperature increased. Apparently, the micrometers
particles exhibit intense green light under 365 nm UV irradiation at
room temperature and no significant decrease in brightness has been Fig. 6. (a) The 3D-TL spectra of LaZn0.7Al11O19:0.3Mn2+. (b) Initial rise anal­
ysis of the corresponding thermo-luminescence glow curves. (c) Schematic
observed even at 450 K. As shown in Fig. 5(b), the emission intensity of
illustration of the mechanism of the quenching process of
LaZn0.7Al11O19:0.3Mn2+ changes little after three cycles of heating and
LaZn0.7Al11O19:0.3Mn2+.
cooling process, indicating that green phosphor met the demand when
applied in a high-power w-LED. Meanwhile, the average decay time
declines about 4.9% points, as shown in Fig. 5(c).
Fig. S5 shows the temperature dependency of Raman spectra of

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Fig. 7. Line-scanning of the PiG sample and the representative EDS mapping images of the as-prepared PiG sample.

LaZn0.7Al11O19:0.3Mn2+ in situ from 290 to 470 K. (a). With increasing

temperature, the Raman peaks shifted towards the long wave numbers,
which was owing to thermal expansion, crystal contraction, phonon
mode contraction, and interlayer coupling. Meanwhile, when the tem­
perature rose, the format of the Raman peak remained same. In addition,
Fig. S5(b) shows the XRD patterns of LaZn0.7Al11O19:0.3Mn2+ as a
function of different testing temperatures, with all diffraction peaks
matching well with the standard card. With the temperature rising from
RT to 520 K, no phase transition or secondary phase found. This in­
dicates that the host, LaZnAl11O19, has a dense skeleton generated by
strong covalent connections between octahedra and tetrahedra, result­
ing in a stiff polyhedral unit. We believe that the structure’s nature
contributes to the minimal luminescence quenching.
In this case, an obvious decline of the PL intensity when the working
temperature over 400 K. It can speculate that other factor may affect the
thermal quenching except for the nonradiative d-d crossover relaxation.
It is generally acknowledged that thermal ionization process occurred
and obviously affect the thermal stability in luminescent materials. The
3D-thermoluminescence (TL) spectra were collected to further investi­
gate the quenching process of LaZn0.7Al11O19:0.3Mn2+. Fig. 6(a) shows
three different TL peaks, which were related to two different trapping
energy levels and black-irradiation. At 400 K, the TL peak corresponds to
a shallow trap, which may confine electrons to a higher excitation en­
ergy level and subsequently release them at lower temperatures. In
Fig. 6(b), the 2D TL spectra correspond to varying shades of tapping Fig. 8. EL spectrum and the related parameters of w-LED device fabricate the
energy levels and the shallow and deep trap determined to be 0.78 eV commercial InGaN blue chip with the PiG sample under 350 mA. (For inter­
and 1.23 eV, respectively. The thermal quenching should originate from pretation of the references to color in this figure legend, the reader is referred to
thermal ionization upon increasing temperature [39]. The following the Web version of this article.)
graphic in Fig. 6 depicts the process of charging for TL measurement and
thermal quenching caused by thermal ionization (Fig. 6(c)). The elec­ LaZn0.7Al11O19:0.3Mn2+-PiG compared with those of LaZ­
tron in higher d orbitals of the Mn2+ ions may be thermally promoted to n0.7Al11O19:0.3Mn2+ powder (Fig. S7(b)).
the lowest conduction band of the LaZnAl11O19 host, and then trapped The LED with green PiG, red phosphor KSF, and commercial blue
by luminescence killer centers at a high temperature. High temperature emitting InGaN chips was developed in order to test the viability of
benefits detrapping and thermal ionization. synthesized PiG in broad-color gamut display backlights. Fig. 8 shows
the EL spectrum of the manufactured LED devices at 350 mA current,
with photos of the LED devices in the inset. The LED shows a bright
2.4. Performance of PiG-composite w-LED device
white light with a CCT of 4818 K and the Ra reaches 89. Unfortunately,
the luminous efficiency of the sample was 49.2 lm/W, probably caused
A remote-type higher powered w-LED prototype device based on the
by the reduced light extraction for opaquer of the PiG. For comparison,
PiG color converter (1 mm in thickness) with 10 wt percent LaZ­
warm WLED was fabricated by using a commercial KSF and YAG
n0.7Al11O19:0.3Mn2+ phosphor was constructed to execute a proof-of-
phosphor. Driven at 25 mA, the warm WLED has a better optical per­
concept experiment. In EDS line-scanning and area analysis, the as-
formance than the as-fabricated WLED, which has a luminous efficiency
synthesized particle embedded in glass matrix reveals characteristic
of 137.2 lm/W, correlated color temperature of 3585 K, and Ra of 88.1,
indications of Zn, Te for glass host and La, Mn for LaZ­
respectively [40,41]. The calculated color gamut can reach 114% of
n0.7Al11O19:0.3Mn2+, validating their chemical composition (Fig. 7).
NTSC space in CIE 1931 with color coordinate is (0.318, 0.334). The
The XRD pattern was collected and shown in Fig. S6 to validate the
results demonstrate that the PiG is being looked at broadly for potential
phase of LZA PiG. The distinctive diffraction peaks of the as-prepared
high-power LCD backlight display.
PiG clearly resemble those of LaZnAl11O19 powder, with the exception
of the amorphous hump of the glass matrix. Due to the absorption of the
3. Conclusions
glass host (Fig. S7(a)), the PLE spectrum of LaZn0.7Al11O19:0.3Mn2+ PiG
lose the UV band comparing with the powder. Moreover, no obvious
In thi work, the narrow green emission LaZn0.7Al11O19:0.3Mn2+ (at
changes are found in the luminescence property of

5
T. Liu et al.
517 nm) phosphor was effectively created by the typical high-
temperature solid reaction to accomplish the low CCT and high Ra of
w-LEDs. The IQE can be the unit one with a color purity of 76.8% under
450 nm blue light stimulation. The excitation wavelength and
temperature-dependent excitation exhibit outstanding luminescence
with a strong thermal stability. Thermoluminescence spectra were used
to investigate the heat quenching of Mn2+ luminescence in LaZnAl11O19.
To make PiG composites, the LaZnAl11O19:Mn2+ phosphor is mixed with
an inorganic glass matrix. The PiG@KSF used an InGaN chip to build a
high-power w-LED device that has superb luminous properties even
when the operating current is as high as 350 mA. These findings show
that the luminescent layer satisfies the LCD’s specifications.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgements
This work is supported by the National Natural Science Foundation
of China (No.51902226, 52002288), the Natural Science Foundation of
Guangdong Province (No.2019A1515012072, 2022A1515011669), the
Innovation Projects of Department of Education of Guangdong Province
(No. 2020KTSCX153), the research and development fund of Wuyi
University joint Hong Kong-Macao (No. 2019WGALH04, No.
2019WGALH09), and the Natural Science Fund for Colleges and Uni­
versities in Jiangsu Province (No. 22KJD150008).
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.ceramint.2022.10.203.
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