Optical Materials 67 (2017) 25e31

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Optical Materials
journal homepage: www.elsevier.com/locate/optmat

White light generation via up-conversion and blue tone in

Er3þ/Tm3þ/Yb3þ-doped zinc-tellurite glasses
V.A.G. Rivera a, *, F.A. Ferri b, L.A.O. Nunes c, E. Marega Jr. c
a
Facultad de Ciencias Físicas, Universidad Nacional Mayor de San Marcos, Lima, Peru
b
Departamento de Física, Universidade Federal de Sa ~o Carlos, Caixa Postal 676, 13565-905, Sa
~o Carlos, SP, Brazil
c ~o Carlos, USP, Caixa Postal 369, 13560-970, Sa
Instituto de Física de Sa ~o Carlos, SP, Brazil

a r t i c l e i n f o a b s t r a c t

Article history: Yb3þ, Er3þ and Tm3þ triply doped zinc-tellurite glass have been prepared containing up to 3.23 wt% of
Received 27 January 2017 rare-earth ion oxides, were characterized by absorption spectroscopy, excitation, emission and up-
Accepted 20 March 2017 conversion spectra. Transparent and homogeneous glasses have been produced, managing the red,
green and blue emission bands, in order to generate white light considering the human eye perception.
The energy transfer (resonant or non-resonant) between those rare-earth ions provides a color balancing
Keywords:
mechanism that maintains the operating point in the white region, generating warm white light, cool
Tellurite glasses
white light and artificial daylight through the increase of the 976/980 nm diode laser excitation power
Energy transfer
Optical properties
from 4 to 470 mW. A light source at 4000 K is obtained under the excitation at 980 nm with 15 mW,
White light generation providing a white light environment that is comfortable to the human eye vision. The spectroscopic
study presented in this work describes the white light generation by the triply-doped zinc-tellurite glass,
ranging from blue, green and red, by controlling the laser excitation power and wavelength at 976/
980 nm. Such white tuning provokes healthy effects on human health throughout the day, especially the
circadian system.
© 2017 Elsevier B.V. All rights reserved.

1. Introduction based on various thin film deposition techniques [3].

In recent years, solid-state lighting (SSL) holds great global
promise for its environmental and financial benefits since it creates
visible light with reduced heat generation and low parasitic energy
dissipation. SSL-based white light generation has fascinated global
attention in recent years, including a Nobel Prize in physics-2014.
The most commonly used approach in InGaN/GaN light-emitting
diodes (LEDs) is the blue electroluminescence, providing a broad-
band emission in the visible region for color conversion [1,2].
Nevertheless, the challenge with LED for illumination is to obtain
high quality white light, for which two approaches are presently
employed: (i) mixture of red (R), green (G) and blue (B) emissions,
(ii) via ultraviolet (UV)-blue down conversion into a color distri-
bution. Another approximation to obtain white light are the organic
light emitting diodes, also called WOLEDs. Their technology offers
the possibility to manufacture in large surfaces, lightweight, flex-
ible, and white/color light emitting devices by low cost processing
* Corresponding author.
E-mail address: garcia@ursa.ifsc.usp.br (V.A.G. Rivera).
An important factor to consider in the white light generation is
the human eye perception. In this way, correlated color tempera-
ture (CCT) and illuminance level are the two most important fea-
tures of light to be considered [4,5]. It is worth saying that CCT is an
essential factor in learning environments because it supports and
enhances the impact of lighting on users [5]. For instance, an
incorrect CCT of light has harmful effects on human health, such as
eyes strain, or effects on emotions and human circadian system
which further cause loss of productivities [6,7]. In this context, the
black body radiation has the warm white light (WWL)
(CCT ¼ 3000 K), cool white light (CWL) (CCT ¼ 4000 K) and artificial
daylight (DL) (CCT ¼ 6500 K) variations. Lighting sources are usu-
ally quoted in terms of power efficiency (lumens per watt) taking
into account the response of the human eye, which is sensitive to
light only in the visible spectrum (400e700 nm) with a maximum
sensitivity at green light (555 nm). Additionally, CCT is also an
important aspect for human perception. Shamsul et al. reported
that a light source with a CCT ¼ 4000 K was most preferred and
most comfortable in comparison with CCTs of 3000 K or 6500 K [8].
Similar results were also found by Kang et al. [9], Lin et al. [10] and

http://dx.doi.org/10.1016/j.optmat.2017.03.028
0925-3467/© 2017 Elsevier B.V. All rights reserved.
26 V.A.G. Rivera et al. / Optical Materials 67 (2017) 25e31
R. Dangol et al. [11]. Considering this, it can be concluded that
people prefer CWL lighting over DL environment.
Great attention has been given to white light generation from
solid-state materials by controlling the intensities of each RGB
emission, for applications in illumination and color displays
[12e14], for instance. White or colored light can also be obtained
via infrared-to-visible conversion and up-conversion (UC) process
in lanthanide doped materials [15,16], and exhibits extensive ap-
plications in color displays, high density optical data storage and
reading, biomedical diagnostics and optical communications
[17e22], etc. However, the control of the relative intensities of the
RGB colors is critical, since the energy transfer (ET) up-conversion
occurs through the population of excited levels and subsequent
ET between real intermediate states. Furthermore, the excitation
pathway through these excited states is different from other
nonlinear optical processes such as multiple harmonic generations
or multiple photon absorption. Up-conversion has a nonlinear
dependence on incident field intensity (input power) [22,23].
Glass oxides such as TeO2, Bi2O3 and PbO are promising mate-
rials for near-infrared technologies, nonlinear optics, solid-state
lasers, displays and other photonic devices [24e26]. Their capac-
ity to incorporate high concentrations of rare-earth (RE) ions also
makes them suitable candidates for the expansion of active pho-
tonic devices. Besides, a single-pumping scheme is desirable in the
multicolored displays due to significantly decreasing of the oper-
ation cost [27]. In this scenario, several groups around the world are
investigating white light-emission in glasses, based on the control
of the three primary colors through UC. Spectroscopic properties of
fluoride, tellurite and germanium glasses, as well as glass-ceramics
and ZBLAN triply-doped with RE ions were reported in
Refs. [12,16,22,28e32]. The intensities of these UC emission bands
can be tunable by changing the pump power intensity. Notably,
Yb3þeEr3þ is a very efficient system for UC via ET process, giving
rise to NIR-to-VIS light conversion. Here, Yb3þ acts as a donor for
Er3þ ions owing to a larger absorption cross-section around 980 nm
(2F7/2 / 2F5/2, resonant with many commercial laser diodes). Then,
efficient ET to 4I11/2 energy level of Er3þ ion can be achieved. At that
point, Er3þ ions are able to convert (UC process) the NIR light into
blue, green and red light. In addition, Tm3þ ions can produce
intense blue and red UC emissions due to highly efficient non-
resonant ET between the Yb3þ:2F5/2/Tm3þ:3H5 states, and two-
photon (via excitation state absorption e ESA) absorption to
Tm3þ:1G4 state. In this manner, if Yb3þeEr3þeTm3þ are introduced
into the glass matrix, we obtained simultaneously the BGR emis-
sions leading to the white light generation [33,34]. Nevertheless,
the choice of the host matrix is extremely important for the
advance of efficient UC optical devices based on RE doped glasses.
In the emission spectra of the rare earth ions into the different host
matrices, an important role belongs to the electronephonon non-
harmonic interaction, which determines the redistribution be-
tween the radiative and non-radiative ET process. Among the glassy
systems mentioned above, tellurite glasses are the more promising
candidates with the proposal to: (i) offer low-phonon energy, (ii) be
transparent in the VIS and NIR region and (iii) have good envi-
ronmental stability for device operation purpose.
This paper investigates the white light generation via up-
conversion, and the blue resonance, in Er3þ/Tm3þ/Yb3þ-doped
zinc-tellurite glasses through manipulating the dual tone
(Yb3þ:Er3þ and Yb3þ:Tm3þ) with two diode lasers pumping at 976
and 980 nm, separately. The mechanisms of UC and ET among the
RE ions were discussed as well. The UC emission intensity as well as
their corresponding lifetimes have been observed and correlated
with the white light generation. The results indicate an intense
WWL (CCT ¼ 3000 K), a reasonable CWL (CCT ¼ 4000 K) and DL
(CCT ¼ 6500 K) emissions by controlling the laser excitation power
and wavelength, according to the CIE-1931 standards. In this
manner, we can generate a correct CCT of light that provokes
healthy effects on human health (specially, the human circadian
system) throughout the day, since it is possible tuning the white
light by means the laser power. Such wide white light tunability is
obtained due to the considerable ability of this distinctive zinc-
tellurite glass, which makes this bulk glass a promising candidate
for applications in SSL and other active photonic devices.
2. Experimental section
The zincetellurite glass samples were prepared according to the
nominal composition (67-x-y)TeO2e30ZnOe3Yb2O3-xTm2O3-
yEr2O3 (in mol%). Tm2O3 was added at different concentrations
(x ¼ 0.1 and 0.2) and Er2O3 with y ¼ 0.03 as the best nominal
concentrations to achieved the white emission from our samples.
The precursor powders are high purity materials (>3 N). Ten grams
of precursor mixture was first dried in a platinum crucible at 300  C
and then melted at 750 and 800  C for 30 min for each temperature
in a resistive furnace under oxidizing conditions, maintaining a low
flow of high purity oxygen within the furnace chamber (rates of
0.5 L/minute). The melted glasses were then casted in a pre-heated
mold, annealed at 340  C for 5 h and slowly cooled down to room
temperature so that the residual stress induced by the rapid cooling
could be removed. The obtained samples of 2.0  1.0  0.2 cm3
dimensions were finally polished up to achieve optical quality and
flat parallel surfaces required for the optical characterizations.
Absorption spectroscopy was performed by a PerkineElmer
Lambda 900 UV/Vis/NIR spectrophotometer, in the range of
350e1100 nm. Excitation spectra were recorded with a fluorimeter
system. Luminescence spectra were performed using a xenon lamp
centered at 355 and 375 nm. These excitation wavelengths are the
Tm3þ[1D2/3H6] and Er3þ[4G11/2 / 4I15/2] absorption lines,
respectively. Up-conversion spectra were performed using 976 and
980 nm diode lasers, an InGaAs detector and the lock-in technique.
In order to guarantee the reproducibility of the measurements
(emission intensity), they were repeated when the samples were
moved in the laser beam or removed and replaced in the mea-
surement apparatus. Multiple measurements were made. For
measuring the lifetime, the samples were irradiated with the har-
monics of a Nd:YAG laser at 355 nm with a pulse width of 5 ns. The
average lifetime was calculated using the following expression:
R∞
tIðtÞdt
t ¼ R0∞ , i.e., an analysis of continuous distributions lifetimes,
IðtÞdt
0
where IðtÞ is the decay time function. The emission signal was
recorded on the oscilloscope. The optical measurements were
performed at room temperature.
3. Results and discussion
In order to obtain white light generation from the glasses, the
host matrix must be transparent in the visible region
(400e700 nm). For this reason, we choose the binary system zinc-
tellurite (ZT) glass, since the UV transmittance of this host matrix is
below of 400 nm in comparison with other tellurite glasses. The
addition of ZnO modify the tellurite glass structure by creating
more non-bridging oxygen (NBOs) in the network [20,35],
increasing the density of this binary system (ZT with
r ¼ 5.21 ± 0.01 g/cm3) [36]. Additionally, the UV transmittance of
ZnO edge shifts to shorter wavelengths with increasing ZnO con-
tent in tellurite glass [37], with an optical band gap of 2.20 eV and
an ultraviolet optical edge at 365 nm for 30 mol% of ZnO. The glass
transition temperature of this ZT is around 366 ± 2  C [36]. Here,
the studied samples are labeled as ZTY_1t, ZTY_2t, ZTY_3e and
 V.A.G. Rivera et al. / Optical Materials 67 (2017) 25e31 27

ZTY_1t3e, where Y corresponds to 3.0 mol% of Yb2O3, 1t and 2t

represents the 0.1 and 0.2 mol% of Tm2O3, and 3e represent the
0.03 mol% of Er2O3.
Fig. 1 shows the optical absorption spectra in arbitrary units of
the glasses, obtained in the 350e1100 nm wavelength range. The
absorption bands observed are due to the electronic transitions
from the ground state to the Yb3þ, Tm3þ and Er3þ excited states.
The absorption section of the Tm3þ ions subtle increases with the
increment of the Tm3þ ion concentrations (ZTY_1t and ZTY_2t
samples), while the absorption section of the Yb3þ ions remains
constant for all samples, and is clearly dominated by the large ab-
sorption section of Yb3þ ions acting as donors for the Tm3þ and Er3þ
ions. The ZTY_1t3e sample shows all the absorption bands of these
rare-earth ions.
The luminescence spectra in the 400e700 nm range under 355
and 375 nm excitations for all the samples are presented in Fig. 2(a)
and (b), respectively. These excitation wavelengths are on the
3
H6/1D2 and 4I15/2 / 4G11/2 absorption lines. Under 355 nm
excitation, the emission intensity of the ZTY_1t sample is higher in
comparison with the ZTY_2t sample, while the ZTY_3e sample does
not show any band emission due to facts that the cross-section of
the 2G7/2 level is smaller and concentration of Er3þ ions is lower in
this sample. The ZTY_1t3e shows the whole emission bands,
including the Er3þ:[2H11/2þ4S3/2 / 4I15/2] transition that was pro-
duced due to ET of Tm3þ:(1G4)/ Er3þ:[2H11/2], see Fig. 2(a). Under
375 nm excitation, the emission intensity of the ZTY_3e sample is
comparable with the ZTY_1t3e sample, while the ZTY_(1e2)t
sample does not show any band emission. Besides, the ZTY_1t3e
sample does not show any band emission of the Tm3þ ions, i.e., in
this sample we do not have ET processes of Er3þ/Tm3þ ions due to
low concentration of Er3þ ions (0.03 mol%), see Fig. 2(b). Therefore,
the Tm3þ and Er3þ ions act in this glass matrix as donor and
acceptor, respectively, and the best Tm2O3 concentration is 0.1 mol
%, since the ZTY_2t sample shows a concentration quenching in the
emission intensity.
In order to analyze the principles responsible for the emissions
in 450 nm Tm3þ:(1G4/3H6), 548 nm Er3þ:(4S3/2 / 4I15/2), and
650 nm Er3þ:(4F9/2 / 4I15/2), the excitation spectrum of the
ZTY_1t3e sample was measured, see Fig. 3. From the normalized
intensity we can say that the maximum emission intensities are the Fig. 2. Luminescence spectra of the ZT glasses showing the characteristic emission
blue color (centered at 450 nm), green color (centered at 548 nm), bands of Tm3þ and Er3þ, under (a) 355 nm and (b) 375 nm excitations, with their
corresponding transitions for the ground state.
and red color (centered at 650 nm), that could be obtained exciting

the Tm3þ:(1D2 at 355 nm), Er3þ:(4G11/2 at 375 nm), and Tm3þ:(1G4

Fig. 1. Absorption spectra of the ZTY glasses showing the characteristic Yb3þ, Tm3þ and
Er3þ absorption bands, with the corresponding absorption transitions from their
ground state. The spectra are vertically shifted for a better reading.
at 462 nm) levels, respectively. In addition, the green and red
emission can also be obtained under other wavelength excitations
in the visible region, which could contribute with the ET processes
after the up-conversion process.
The emission bands observed in the up-conversion spectra, see
Fig. 4(a) and (b), can be assigned as follows: (i) the 479, 527, 548,
659 and 670 nm bands are originated from the Er3þ radiative
transitions from the excited states 4F7/2, 2H11/2, 4S3/2, and 4F9/2 to the
ground state 4I15/2, respectively, and (ii) the 477 and 651 nm bands
are due to Tm3þ direct radiative transitions from the excited states
1
G4 and 3F2,3 to the ground state 3H6, respectively, while the 694 nm
band corresponds to indirect transitions from the excited state 1G4
to the excited state 3F4. The power pumping employed to excite the
samples in both Fig. 4(a) and (b) corresponds to the maximums of
976 and 980 nm of the diode laser, respectively. One can determine
the peak rate among the blue emission against the green or red
emission (lp¼479/lp¼548 and lp¼479/lp¼659) under different diode
lasers for the TZY_1t3e sample. Under 976 nm excitation we have
lp¼479/lp¼548 ¼ 2.03 and lp¼479/lp¼659 ¼ 3.14, under 980 nm
excitation we have lp¼479/lp¼548 ¼ 3.41 and lp¼479/lp¼659 ¼ 6.58.
28 V.A.G. Rivera et al. / Optical Materials 67 (2017) 25e31

Fig. 3. Excitation spectrum of the ZTY_1t3e sample, showing the principles respon-
sible for the Red, Green and Blue (RGB color) emissions. (For interpretation of the
Fig. 5. Decay lifetime (normal scale) of the 450, 540, 651 and 670 nm emission bands
references to colour in this figure legend, the reader is referred to the web version of
under excitation at 355 nm for all the prepared samples.
this article.)

We can see that the blue up-conversion emission is selective to the harmonic is at 490 nm, which is near of the Er3þ:(4F7/2e489 nm),
wavelength excitation. The conversion of 980 nm to its second- see Fig. 1. In addition, the Er3þ:(4F7/2) level can populate the

Fig. 4. Up-conversion emission spectra of the samples under (a) 976 nm and (b) 980 nm excitation laser. Up-conversion emission spectra of the TZY_1t3e sample as a function of
laser diode pump power at (c) 976 nm and (d) 980 nm. Inset: logelog plot of the emission intensity as a function of excitation power extracted from figures (c)e(d).
 V.A.G. Rivera et al. / Optical Materials 67 (2017) 25e31 29

Fig. 6. (a) Energy level of Yb3þ, Er3þ and Tm3þ, and transition pathways, and (b) CIE (x,y) chromaticity diagram showing the color coordinates of the white light up-conversion
tunability in the ZTY_1t3e glass. The images presented in Figures 6 (c)e(g) are photographs displaying the different colors emitted by the glasses prepared here. ZTY_1t3e
sample under 980 nm with (c) 350 and (d) 15 mW pump power. (e) ZTY_3e sample under 980 nm and 350 mW. ZTY_1t sample under (f) 980 and 350 mW and (g) 976 nm and
470 mW. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Tm3þ:(1G4) level via multipolar interaction, resulting in an increase
of the blue emission intensity of the TZY_1t3e sample. The excita-
tion spectrum centered at 548 nm shows that the 487 nm is the
second responsible for the emission green, and can provoke the red
emission, see Figs. 2 and 3. Therefore, the blue up-conversion
emission favors both green and red emissions.
In the same way, the up-conversion emission spectra in the
range of 400e750 nm of the ZTY_1t3e glass are presented in
Fig. 4(c) and (d) under 976 and 980 nm excitations, respectively, as
well the dependence on the pump power of the maximum in-
tensity of the bands centered at 479, 526, 548, 659 and 694 nm. The
up-conversion emission intensity IUC is proportional to the nth
pump power P as IUC fPn , where n accounts for the number of
excitation infrared photons involved in the excitation mechanism
(photons absorbed per up-converted emitted photons). The num-
ber n is necessarily an integer and is obtained from the slope of the
straight line obtained by plotting logarithmic of P(IUC ), see insets of
Fig. 4(c) and (d). The regression curves were obtained with an R2
value higher than 0.99, as shown by the standard error values
determined for each slope and displayed in the respective legends.
Therefore, the TZY_1t3e sample generates white light by means of
the following processes: (i) the blue emission intensity exhibits
three-photon, indicating that three photons are involved in the
population inversion in both cases, see Fig. 4(c) and (d); (ii) the
green (526 and 548 nm) emissions are related to a two-photon
under 976 and 980 nm excitations; (iii) the attribution of the red
30 V.A.G. Rivera et al. / Optical Materials 67 (2017) 25e31
emission observed at 635e680 nm is ambiguous because both Er3þ
and Tm3þ ions may emit in this region, i.e., Er3þ:(4F9/2 / 4I15/
3þ 3 3
2) þ Tm :( F2/ H6), see Fig. 4(a) and (b); and (iv) the red emis-
sion at 694 nm can be unambiguously ascribed to the
Tm3þ:(3F3/3H6). Higher P increases the competition between the
linear/intermediate decay and up-conversion processes, due to the
share of the intermediate excited states Er3þ:(4F7/2 / 4I13/2, 2H9/
4 3þ 1 3
2 / I11/2) and Tm :( D2/ H4), resulting in a depletion of the n
power for the peaks, see insets of Fig. 4(c) and (d), with a slope ~ 3.
Thereby, it is possible to obtain three-photons for the red emission
at 694 nm.
The decay lifetimes for the samples, measured at four emission
wavelengths, 479, 548, 659 and 694 nm, by exciting at 355 nm, are
plotted in Fig. 5. The lifetimes measured for the blue, green and red
transitions were identified as above. The energy transfer between a
donor and an acceptor (between rare-earth ions) can be studied via
Foster's interaction [38], and characteristic features of this coupling
are changes in the decay lifetime. In this way, at 479 nm, the ZTY_1t
and ZTY_2t samples show practically the same values lifetime, but
the ZTY_1t3e sample exhibits a low decrease in comparison to the
other samples. Therefore, it is expected an resonant ET from the
Tm3þ to Er3þ. At 548 nm, a decrease of the lifetime is observed in
the ZTY_1t3e sample in comparison with the ZTY_3e sample.
Therefore, we have an non-resonant ET from the Er3þ to Tm3þ. A
similar effect is also observed at 659 nm. At 694 nm, a decrease of
the lifetime is observed in the ZTY_1t3e sample in comparison with
the ZTY_1t sample. Therefore, we have an resonant ET from the
Tm3þ to Er3þ. The absorption of the 976/980 nm laser by the Yb3þ
and Er3þ ion enables the excitation of the 4I11/2 metastable level and
consecutive excitations of blue color (both Er3þ and Tm3þ), through
an ESA and two-photons absorption. Then, non-radiative processes
enable the excitation of consecutive energy levels through ET
(resonant or non-resonant), as shown in Fig. 6 (a).
In this color-converting ZTY_1t3e glass after up-conversion
process, the ET is exclusively a result of the dipoleedipole inter-
action between the Tm3þ/Er3þ ions. Here, the ET provides a color
balancing mechanism that maintains the operating point in the
white region, at the same time as it also shifts the coordinates to-
ward a warmer color temperature due to the diode laser (wave-
length and power pump), see Fig. 6(b)e(g). The chromaticity
diagram presented in Fig. 6 (b) shows the white light tuning ob-
tained from the ZTY_1t3e glass by increasing the 976/980 nm laser
diode excitation power from 4 to 470 mW [see also Fig. 4(c) and
(d)], as indicated for each sample. The observed white light has CIE
coordinates of (0.33, 0.33). Also, there is a quite broad region of the
diagram around this point that can be considered white light under
both laser diodes, see the CCT line. Additionally, a light source with
a CCT ~4000 K is obtained under laser diode excitation at 980 nm
with 15 mW, providing us a CWL lighting environment that is
comfortable for the human eye vision. The images presented in
Fig. 6(c)e(g) are photographs showing the different colors emitted
by the glasses prepared in this work.
4. Conclusions
In summary, Yb3þ, Er3þ and Tm3þ triply doped zinc-tellurite
glasses have been prepared in view of producing white light by
means of the blue tuning consisting in a mixture of red, green and
blue (RGB) emission bands of the rare earth ions via an excitation in
the near infrared range (at 976 and 980 nm). The optimal rare-earth
ion concentrations to achieve this aim were 3 wt% of Yb2O3, 0.03 wt
% of Er2O3 and 0.1 wt% of Tm2O3. Then, highly transparent and
optically homogeneous zinc-tellurite glasses have been fabricated
through the appropriate choice of selected compositions near their
glass transition temperatures. Significant changes in the relative
intensity of the blue, green and red emissions upon 976/980 nm
laser diode excitation have been observed as a function of the
wavelength and power of the applied laser excitation. Such feature
is attributed to the tuning of Yb3þ ions under 976/980 nm excitation
which gives rise to a wide range of white light [warm white light (at
3000 K), cool white light (at 4000 K) and artificial daylight (at
6500 K), according to the CIE-1931 standards] by only controlling
the laser excitation power of the zinc-tellurite glass. Such extensive
emission tunability via energy transfer between those rare-earth
ions makes these materials promising candidates for applications
in solid-state lighting, solar cell technology and other active pho-
tonic devices.
Acknowledgments
This work was supported by the Brazilian agencies Capes,
FAPESP and CNPq through the INOF/CEPOF (Instituto Nacional de

Optica e Foto 
^ nica and Centro de Pesquisa em Optica ^nica e
e Foto
S~
ao Paulo e Brazil).
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