JOURNAL OF RARE EARTHS, Vol. 29, No. 5, May 2011, P.

420

Saturation effect of up-conversion luminescence from erbium-doped, silica-

titania sol-gel powders
Jesús Castañeda
(Guadalajara University, Los Lagos University Center, Enrique Diaz de León St., 1144. Lagos de Moreno, Jalisco, 47460 Mexico)

Received 12 October 2010; revised 15 December 2010

Abstract: The intensity of the visible up-conversion luminescence could be limited by a saturation effect produced by increased pump power.
Visible up-conversion luminescence was obtained in erbium doped, silica-titania sol gel powders under dynamical pumping at 1532 nm. The
saturation effect was studied for erbium radiative transitions 2H9/2ĺ4I15/2 (410 nm), 2H11/2ĺ4I15/2 (530 nm), 4S3/2ĺ4I15/2 (550 nm), 2H9/2ĺ4I13/2
(567 nm) and 4F9/2ĺ4I15/2 (675 nm). The recorded up-conversion luminescence decreased when increasing excitation power. The results sug-
gested that the saturation effect was determined by the pump power, the sample composition and the lifetimes of the corresponding first ex-
cited states.

Keywords: erbium; up-conversion; luminescence saturation; rare earths

Currently, materials doped with rare earths find usage in a
wide variety of applications, including phosphors, monitors,
X-ray imaging, lasers, and amplifiers for fiber-optic com-
munications. Therefore, a great deal of research on IR-to-
visible frequency up-conversion in erbium-doped materials
is in progress because of their unique spectral properties, in-
cluding multiple emissions in visible region, when exciting
the ions at lower energy wavelengths, i.e. near infrared. Sev-
eral reports have shown this for optical waveguides[1–4],
glasses[5–7] and crystals[8]. Up-conversion luminescence
opens the possibility for the fabrication of visible lasers, low
intensity IR imaging, hot emission and avalanche like
co-doped systems and biological applications[9]. The pre-
dominant mechanisms of up-conversion in these materials
are excited-state absorption (ESA) and energy transfer[10–12].
The luminescence intensity from ESA processes is inde-
pendent of erbium content, whereas up-conversion emissions
due to energy transfer processes are increased for higher er-
bium content, and when the distance among Er3+ is reduced
as a consequence of cluster formation[13–15]. Therefore, up-
converted luminescence intensity depends mainly on erbium
content, host composition and pump power. However, the
luminescence intensity is limited by a saturation effect[16].
The physical explanation for this saturation is attributed to
several factors, such as the enhancement of energy transfer
rates due to high concentration of rare earth ions[17] and the
depletion of ground state population[18]. Another proposal is
a competence between energy transfer processes and no ra-
diative decays in the depletion of intermediate excited
states[19]. Most saturation studies are solely based on the 550 nm
erbium emission[20–22] because of its higher intensity, and to
the best of our knowledge this may be the first experimental
report of the saturation effect for the erbium emissions at 410,
530, 567 and 675 nm under pulsed excitation.
1 Experimental
Sol-gel binary glasses of silica-titania (SiO2-TiO2) have
been used in the fabrication of optical waveguides devices,
and have proven to be suitable for incorporating erbium
ions[1]. Erbium doped, SiO2-TiO2 sol-gel powders at different
TiO2 molar ratios were prepared as described in Ref. [23].
All chemicals were of reagent grade, and utilized without
further purification. Erbium ions were obtained from erbium
chloride (Aldrich). SiO2 and TiO2 precursors were tetraeth-
oxysilane (Aldrich) and titanium isopropoxide (Chemat),
respectively. The obtained samples were fired in air atmos-
phere at 500 °C for 24 h. The Er3+ molar ratio was fixed at
10%; whereas the TiO2 molar ratios were 10%, 25%, 50%
and 70%. The crystalline phases of the powders were identi-
fied by X-ray diffraction (XRD), with a Rigaku diffractome-
ter coupled with a Cu source at 40 kV. A pulsed MOPO-SL
system from Spectra-Physics was the excitation source in the
Er3+ luminescence studies. It had a pulse width of 10 ns, with
a 10 Hz pulse rate. The light spot area was about 3–5 mm2.
The luminescence from the samples was dispersed with a
spectrograph Spectra-Pro 500 from Acton-Research. A
Molectron EPM2000 power meter was utilized to measure
and average the incident pump power over the dwell time of
the acquisition. The error on these measurements was esti-
mated at 5%.
2 Results and discussion

Corresponding author: Jesús Castañeda (E-mail: jcc050769@yahoo.com.mx; Tel.: +52-1-474-742-3678)

DOI: 10.1016/S1002-0721(10)60472-3
Jesús Castañeda, Saturation effect of up-conversion luminescence from erbium-doped, silica-titania sol-gel powders
2.1 DRX study
Fig. 1 shows the XRD of a SiO2-TiO2-Er3+ sample at 10%
3+
Er and 25% TiO2 molar ratios. The peaks of the XRD pat-
tern are related to anatase phase (PDF 21-1272). No peaks
from erbium oxide were observed as in Refs. [24,25]. How-
ever, it is expected that the rare earth exists as Er3+, due to
the erbium incorporation in the crystalline host. Thus the er-
bium ion would exhibit intense narrow-band luminescence
in our SiO2-TiO2 matrix. The relatively low intensity diffrac-
tion peaks confirms that the sample is partially crystalline.
The grain size in the sample was ~11 nm, as estimated using
the Scherrer equation in the 101 direction.
2.2 Up-conversion luminescence under 1532 nm excita-
tion of SiO2-TiO2-Er3+ powder
The up-conversion spectrum obtained upon 1532 nm ex-
citation is shown in Fig. 2 for a SiO2-TiO2-Er3+ sample at
25% TiO2 molar ratio. The high erbium content suggests that
energy transfer in samples was the main population mecha-
nism of Er3+ excited states[5,14,15]. The depicted spectrum had
several emissions, such as emission band centered at 410 nm,
attributed to 2H9/2ĺ4I15/2 transition. A proposed excitation
path is shown in Fig. 3(a). The emission at 530 nm is attrib-
uted to 2H11/2ĺ 4I15/2 transition. The next emission at 550 nm
is due to 4S3/2ĺ4I15/2 transition. There is a shoulder located at
567 nm which is produced from 2H9/2ĺ4I13/2 transition. The
Fig. 1 XRD pattern of the SiO2-TiO2-Er3+ sample with 10% Er3+
and 25% TiO2 molar ratios
Fig. 2 Up-conversion spectrum of SiO2-TiO2-Er3+ powder at 10%
erbium content and 25% TiO2 when excited at 1532 nm
421
Fig. 3 Simplified energy-levels diagram of Er3+ and up-conversion
paths for the Er3+ green and blue emissions bands at 1532 nm
excitation (a), the Er3+ red emission obtained under 1532 nm
excitation (b), an alternative population mechanism for 2H9/2
excited state (c)
spectra also show a red emission located at 675 nm, pro-
duced from 4F9/2ĺ4I15/2 transition. However, no emission
was obtained at 800 nm (from 4I9/2ĺ4I15/2 transition), simi-
larly to that report by Amorim et al.[5] for an Er3+ doped
chalcogenide glass. Nevertheless, the 800 nm emission is
observed on other hosts, such as on Er3+ doped fluoride
glasses[17], erbium-doped fluorozirconate glasses[26] and on
erbium-implanted Al2O3 waveguides[15].
The up-conversion process depends on the lifetimes of the
intermediate excited levels, which are determined by the ra-
diative constants and multi-phonon transitions[27]. At 1532
nm excitation, the Er3+ first excited level is 4I13/2, as shown in
Fig. 3(a). This state has a long lifetime[28], which gives
closely spaced erbium neighbors plenty of time to interact
and populate the next excited state 4I9/2, through the energy
transfer process (4I13/2+4I13/2)ĺ(4I9/2+4I15/2).
No emission was detected from 4I9/2, probably as a result
of a strong 4I9/2ĺ4I11/2 multi-phonon relaxation. The inter-
mediate level 4I9/2 is strongly affected by multi-phonon decay,
because this level has the smallest energy gap to the next
lower-lying level, 4I11/2. The average 4I9/2ĺ4I11/2 energy gap
is reported at ~1890 cm–1 for oxide-based materials[10],
which implies an average of three phonons to bridge the
aforementioned gap. Therefore, the 4I9/2 lifetime is expected
to be further decreased when Er3+ is added to the SiO2-TiO2
host, but the recorded luminescence from 4S3/2ĺ4I15/2 transi-
tion suggests that 4I9/2ĺ4I11/2 multi-phonon relaxation is
probably suppressed to some extent. A similar behavior was
reported by Hehlen et al.[29] for a decrease of multi-phonon
relaxation in ZBLAN:Er3+ glasses. It is proposed that multi-
phonon decay is inhibited due to the proximity among Er3+
in our highly doped sample, thus the energy transfer process
(4I9/2+4I13/2)ĺ(2H11/2-4S3/2+4I15/2) is feasible to occur, as
shown in Fig. 3(b). This mechanism depleted 4I9/2 and popu-
lated the manifold 2H11/2–4S3/2, producing a relatively high
population density for the latter levels. In addition, the
short 4S3/2 lifetime (~1 μS on an oxide based matrix) and
422 JOURNAL OF RARE EARTHS, Vol. 29, No. 5, May 2011

the large band-gap to the next lower-lying level 4F9/2 pro-
moted a significant decay mechanism through the radiative
transition 4S3/2ĺ4I15/2. Although there are several up-con-
version processes that could populate 4S3/2, just two addi-
tional mechanisms such as ESA (4I9/2+absorption of a 1532
nm photon), and the energy transfer (4I11/2+4F9/2)ĺ
(4I13/2+4S3/2) were considered as alternative processes to
populate 4S3/2 excited state[30]. However, these processes
were discarded because the former mechanism is independ-
ent of the erbium concentration and the latter is better suited
to populate 4F9/2 excited state[10] in form of cross relaxation
(4I13/2+4S3/2)ĺ(4I11/2+4F9/2), as shown in Fig. 3(b). This four-
photon process is expected to be supported on samples doped
at high erbium content and explains the recorded 675 nm emis-
sion. On the other hand, a proposed path to populate the
level 2H9/2 is through the four-photon sequence 4I15/2ĺ
4
I13/2ĺ4I9/2ĺ4S3/2ĺ2H9/2 thus originating a weak blue emis-
sion at 410 nm and a green emission at 567 nm, although the
short lifetime of intermediate state 4S3/2 is a potential drawback
for 2H9/2 population. Another mechanism to populate 2H9/2 is
through the absorption of a 550 nm photon by meta-stable
state 4I13/2, as shown in Fig. 3(c). This three-photon process
could lead to the 2H9/2 excited level population and hence to
the aforementioned emission bands at 410 and 567 nm.
populate 2H11/2 excited state is through a three-photon proc-
ess: 4I15/2ĺ 4I13/2ĺ 4I9/2ĺ2H11/2; therefore, a slope of three
was expected. However, as shown in Fig. 4, the 530 nm
emission has an initial slope of 2.4, and then decreases to 1.8
for increasing pump power. A similar behavior was obtained
for the green emission at 567 nm, which was produced from
a three photon process: it started with a slope of 2.6, and then
decreased to a value of 2.0 for increased pump power.
The corresponding slopes of 410 and 567 nm were quite
similar, suggesting a three-photon population mechanism for
2
H9/2 excited state. Finally the red emission (675 nm), which
was produced from 4F9/2ĺ4I15/2 radiative transition, had an
initial slope of 3.6 for low pump power, thus decreasing to a
slope value of 1.7 when pump power was increased. To ex-
plain the recorded saturation behavior, a simplified four level
system is proposed in Fig. 5 to populate 2H11/2, where N0, N1,
N2 and N3 are the populations of the corresponding excited
states; P is the pumping intensity; A1, A2 and A3 are the de-
population processes to the ground state, and finally U1 and
U2 are energy transfer terms.

2.3 Visible luminescence saturation of Er3+ under 1532

nm excitation
The slope of the dependence of luminescence versus
pump power in a double logarithmic plot is supposed to pro-
vide the number n of pump photons required to populate an
emitting state. However, this behavior can be questioned in
some practical cases, as reported by Mita et al.[31] for Ho3+
Yb3+ co-doped oxyfluoride glass, where the slopes of the
curves of up conversion luminescence vs. pumping power Fig. 4 Log-log plot of up-conversion visible emissions intensity
are smaller than normal multi-photon relaxation. Similar re- versus 1532 nm pump power for SiO2-TiO2-Er3+ samples at
sults were reported in Er3+ doped chalcogenide glass[5], Er3+ 10% erbium content (The TiO2 content of the samples is
doped fluorozirconate glasses[26] and in Cs3Lu2Cl9:1% Er3+, 25%; the numbers on the plot denote the measured slopes at
Cs3Er2Cl9 crystals[19]. To explain this saturation behavior, low and high pump powers, respectively)
Pollnau et al.[19] suggested that there is a competence be-
tween up conversion processes and natural decays on the de-
pletion of Er3+ intermediate states under continuous excita-
tion. When the slope is near the number n of pump photons
required to populate an emitting state, it is an indication that
intermediate levels are depopulated mainly by natural decay
to the ground state. On the other hand, when up conversion
processes play an important role in intermediate states deple-
tion, a slope value smaller than n is obtained on the corre-
sponding plot. Most saturation studies are related to Er3+
up-conversion emission at 550 nm. The probable reason is
the large intensity from 4S3/2ĺ4I15/2 radiative transition,
which is often higher than other Er3+ visible emission bands.
In order to get a broader knowledge of the visible lumines- Fig. 5 Simplified four-level system related to Er3+ excited states (P
cence saturation, this work focused instead on the visible is the pump power, Nn are the populations of the corre-
up-conversion emissions at 530, 410, 567 and 675 nm. The sponding excited levels, An are related to the depopulation
former emission is due to the radiative transition 2H11/2ĺ processes and Un are the energy transfer terms)
4
I15/2, as stated in section 2.2. The up-conversion path to
Jesús Castañeda, Saturation effect of up-conversion luminescence from erbium-doped, silica-titania sol-gel powders 423

The rate equations describing the corresponding mecha-

nisms are:

(1)

(2)

(3)

The energy transfer was supposed as the dominant popu-

lation mechanism, due to the high erbium content in our
samples. Eqs. ((1)–(3)) are simplified under steady state ex-
citation as in Ref. [19], obtaining the expression N3 v P (4),
where N3 is related to 2H11/2 and P is the pump power. A
concordance of expression (4) to the experimental results is
noticed, i.e., the slope values are lower than the order of the
up-conversion process. Therefore, the slope from 2H11/2 is
expected to converge to one for increased pump power. This
condition is approximately fulfilled on the 1.8 slope value
shown in Fig. 4 for 530 nm emission, although the pump
power dependence seems to be rather P3/2 than P1. This is
probably due to the weakness of our excitation source, pre-
venting higher saturation from occurring. With an increase in
the excitation intensity, a saturation on the absorption of the
excited states is expected. By further increasing the pump
power, a saturation of the up-conversion luminescence is
expected due to the depletion of the ground state. The latter
is due to the long lifetime of the first excited state (4I13/2),
which is separated by a large energy gap from the ground
state[28], so its lifetime is very long. This lifetime favors the
population of higher excited states by energy transfer proc-
esses, thus reducing the ground state population to some ex-
tent. Although we failed to measure the 4I13/2 lifetime in our
samples, it is reported at around 10 ms for a silica-titania
host[28]. On the other hand, if we consider the decay to the
ground state as the dominant depletion mechanism of inter-
mediate states, then the expression N3 v P3 is obtained from
rate Eqs. ((1)–(3)). The corresponding cubic slope is almost
accomplished at low pump power for the 530 nm emission
(Fig. 4). These assumptions could be extended to the other
Er3+ excited states and thus explained the slope value of 3.6
obtained for the 675 nm emission al low pump power: a
four-photon process is expected in the population process of
4
F9/2 excited state, as stated in section 2.2. The proposed
model, although obtained under steady state excitation
schemes, explains the experimental results rather well de-
spite the utilized dynamical pumping and the lack of pump
power.
Fig. 6 Up-conversion spectra of SiO2-TiO2-Er3+ samples excited at
1532 nm (The TiO2 contents of the samples were 10 % and
70%, whereas the corresponding Er3+ content was fixed at
10%)
nescence intensity is quenched for increased TiO2 content.
The up-conversion mechanisms for these emissions were
described previously in section 2.2.
On these results, the recorded luminescence intensity con-
firms that energy transfer processes depend on the concen-
tration of the active ions and on the relative distances among
them: it is well known that at low concentrations of TiO2, the
formation of Er3+ clusters is expected to occur[32], allowing
energy transfer processes to have major importance on the
up-conversion process. Therefore, the saturation effect due
to the depopulation of the first excited state is feasible, as
explained in section 2.3. On the other hand, when increasing
TiO2 content, the erbium ions got more separated and neither
energy transfer processes nor saturation effect were favored
to occur. The later assumptions were reinforced with the
measured slopes for the 550 nm emission, as shown in Fig. 7.
The slope for the sample at 10% TiO2 content was 2.0 for
low pump energy, decreasing to 1.3 for higher excitation
power. For the 50% TiO2 sample, the measured slopes were
2.8 and 2.1 for low and high pump power; whereas, the cor-

2.4 Up-conversion on SiO2-TiO2-Er3+ samples with a

fixed Er3+ content
In order to support the latter assumptions, a set of three
SiO2-TiO2-Er3+ samples with different TiO2 contents were
excited at 1532 nm. The corresponding TiO2 molar ratios of
these samples were 10%, 50% and 70%. The corresponding
up-conversion spectra are shown in Fig. 6, where the lumi
Fig. 7 Log-log plot of up-conversion visible emissions intensity
versus pump power for SiO2-TiO2-Er3+ samples at 10%,
50% and 70% TiO2 content (The erbium content of the sam-
ples is fixed at 10%; the numbers on the plot denote the
measured slopes at low and high pump powers, respectively)
424
responding slopes for the 70% TiO2 sample were 3.0 and 2.4
for low and higher pump power, respectively. This saturation
behavior could be explained as in section 2.3, where a de-
crease in the slope indicates a dominance of energy transfer
processes on the depletion of 4I13/2 excited state, and slope
values close to n are related to depletion of intermediate
states by decay to the ground state. Although the results in
the present section were only based on three samples at dif-
ferent TiO2 contents, the wide range on the TiO2 content
(10%–70%) and the recorded saturation behavior confirmed
that the depopulation of 4I13/2 excited level, which is driven
by energy transfer processes and non radiative decays, is an
important factor for the recorded luminescence saturation
due to increased pump power.
3 Conclusions
Visible up conversion luminescence was obtained from
SiO2-TiO2-Er3+ sol-gel powders excited at 1532 nm. The
measured slopes of the log-log plots of visible luminescence
intensity versus pump power had a dependence on pump
power. At 1532 nm excitation, the observed saturation of
visible emissions was due to the long lifetime of 4I13/2 excited
state that produced ground state depopulation when increas-
ing pump power.
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