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J64 Electrochemical and Solid-State Letters, 12 共7兲 J64-J68 共2009兲
1099-0062/2009/12共7兲/J64/5/$25.00 © The Electrochemical Society

Fluorescence Properties of Nd3+-Doped KNbO3 Phosphors

R. Balakrishnaiah,a,b Dong Woo Kim,a Soung Soo Yi,a,z Kwang Duk Kim,c
Sung Hoon Kim,c Kiwan Jang,b Ho Sueb Lee,b and Jung Hyun Jeongd
a
Department of Electronic Materials Engineering and cDepartment of Engineering in Energy and Applied
Chemistry, Silla University, Busan 617-736, Republic of Korea
b
Department of Physics, Changwon National University, Changwon 641-773, Republic of Korea
d
Department of Physics, Pukyong National University, Busan 608-737, Republic of Korea

Nd3+-doped potassium niobate 共K共1−x兲NbO3:Nd共x兲 3+

兲 polycrystalline powder phosphors for x = 0.01, 0.03, 0.05, and 0.07 mol were
prepared by the conventional solid-state reaction method and were characterized by X-ray diffraction 共XRD兲, field-emission-
scanning electron microscopy, transmission electron microscopy, and photoluminescence measurements. The XRD data have
shown a single-phase orthorhombic structure for x = 0.01 and 0.03 mol concentrations of Nd3+ ions, while an additional NdNbO4
phase is observed at higher concentrations. The photoluminescence spectrum has shown an intense emission band at 1061 nm
along with two weak emission bands at 881 and 1343 nm when the samples are excited with 514.5 nm radiation of an Ar+-ion
laser. No drastic changes in the intensity of emissions are observed with concentration variation, except slight changes in the
intensities and peak positions of crystal-field peaks.
© 2009 The Electrochemical Society. 关DOI: 10.1149/1.3125273兴 All rights reserved.

Manuscript submitted November 25, 2008; revised manuscript received April 7, 2009. Published April 29, 2009.

Research interest on lanthanide 共Ln兲-doped materials is rapidly as KNN01, KNN03, KNN05, and KNN07, respectively. The crystal
growing due to their potential applications as nonlinear optical ma- structures of the prepared samples were examined by X-ray diffrac-
terials. These materials found wide use in the development of tion 共XRD兲 analysis using a high resolution XRD system with
plasma display panels, field emission displays, and electrolumines- Cu K␣1 radiation 共␭ = 1.542 Å兲. The surface morphologies of the
cent panels. Many researchers reported various phosphor host ma- samples were investigated by the field-emission-scanning electron
trices with suitable luminescent Ln ions that found vital applications microscopy 共FESEM兲 images using a field-emission gun scanning
in optical devices such as fluorescent lamps, cathode ray tubes, and electron microscope 共JSM-6700F兲 operated at 15 kV, which also
X-ray intensifying screens.1-5 Potassium niobate 共KNbO3兲 is recog- provided the energy-dispersive analysis through its integrated
nized as one of the best host matrices for Ln ions as it is a useful energy-dispersive X-ray spectrometer 共EDXS兲 to analyze the com-
candidate for ferroelectric materials with excellent electro-optic and positional molar ratios. The particle sizes were analyzed through
nonlinear optical coefficients, which have attracted a great interest transmission electron microscopy 共TEM兲 images also using a trans-
for applications in optical waveguides, frequency doublers, and ho- mission electron microscope 共JEM-2010 JEOL, H-7500 Hitachi兲.
lographic storage systems.6,7 Among Ln ions, Nd3+ ion is one of the The NIR emission spectra 共800–1600 nm兲 were measured at room
most extensively studied ions for solid-state lasers due to its laser temperature on exciting the samples by the 514.5 nm wavelength of
emission at a very useful wavelength, 1064 nm, in addition to the an Ar+-ion laser using a fluorescence spectrophotometer connected
possibility of lasing at other wavelengths such as 1800, 1350, and to a computer-controlled EC&G Princeton Applied Research 5207
881 nm at room temperature. Also, its absorption in the UV–visible– lock-in amplifier. The signal was then analyzed using a 0.5 m mono-
near-IR 共NIR兲 regions allows an efficient pumping either with chromator equipped with a 150 lines/mm grating and detected with
broad-band sources 共Xenon lamp兲 or with sources of selected wave- an InGaAs PMT and a digital oscilloscope.
length using diode lasers.8,9 Although plenty of articles on various
preparation methods and structural investigations of KNbO3-related Results and Discussion
perovskite ceramics are available,10-17 only a few articles18-24 can be The XRD patterns of the prepared samples are shown in Fig. 1.
found on the luminescent characterization of Ln-doped perovskite As can be seen in Fig. 1, for the KNN01 sample, the diffraction
materials. Therefore, based on this motivation, we have prepared the
KNbO3:Nd3+ phosphors with different concentrations of Nd3+ ions
by the conventional solid-state reaction method in our present work,
and the dependence of morphological and fluorescence properties of
the prepared materials on Nd3+-ion concentration has been investi-
gated.

Experimental
3+
The Nd -doped KNbO3 powder phosphors were synthesized by
the conventional solid-state reaction method by using the raw mate-
rials of high purity chemicals: K2CO3 共99.9%, Aldrich兲, Nb2O5
共99.9%, Aldrich兲, and Nd2O3 共99.99%, Alfa兲. These raw materials
with correct proportional amounts were finely ground in an agate
mortar with a pestle on adding a little amount of acetone. The mix-
ture was then taken in an alumina crucible, sintered in a tubular
electric furnace at 120°C for 1 h, 750°C for 4 h, and 1050°C for 4
h, and finally annealed at 400°C for 10 h at ambient atmosphere.
3+
The concentrations of Nd3+ ions doped in the K共1−x兲NbO共3+␦兲:Nd共x兲
共KNN兲 phosphors were taken as x = 0.01, 0.03, 0.05, and 0.07 mol,
and here afterward, for simplicity, these samples have been labeled

Figure 1. XRD patterns of 共a兲 0.01, 共b兲 0.03, 共c兲 0.05, and 共d兲 0.07 mol
z
E-mail: ssyi@silla.ac.kr concentrations of Nd3+-doped KNbO3 phosphors, along with JCPDS data.
 Electrochemical and Solid-State Letters, 12 共7兲 J64-J68 共2009兲 J65

peaks are observed at the diffraction angles 2␪ of 22.05 共110兲, 22.30

共001兲, 31.55 共111兲, 44.95 共220兲, 45.60 共002兲, 50.75 共221兲, 51.20
共112兲, 56.00 共311兲, 56.40 共022兲, and 65.95 共222兲; the same are ob-
served for KNN03, KNN05, and KNN07 samples. The intensities
and positions of these diffraction peaks are consistent with the the-
oretical diffraction data of KNbO3 共JCPDS Card no. 32-0822兲, in-
dicating the good formation of the KNbO3 composite material with
the substitution of Nd3+ ions into the K+ sites.24 This also agrees
with the compositional molar ratios nearer to 共K + Nd兲:Nb:O
⬇ 1:1:3 according to the compositional formula
3+
K共1−x兲NbO共3+␦兲:Nd共x兲 , as observed from EDXS analyses. The molar
ratios of 共K + Nd兲:Nb:O:Nd observed from the EDXS analyses are
1.00:1.09:2.80:0.04, 1.00:1.08:2.55:0.05, 1.00:1.10:3.19:0.06, and
1.00:1.12:2.54:0.09 for the KNN01, KNN03, KNN05, and KNN07
samples, respectively. As can be seen in Fig. 1, all the samples are
found orthorhombic in structure because of the split of the diffrac-
tion peaks, 共220兲 and 共002兲.16,18,19 According to earlier studies,18-21
KNbO3 phosphor undergoes phase transitions from rhombohedral to
orthorhombic at −10°C, from orthorhombic to tetragonal at 225°C,
and finally from tetragonal to cubic at 435°C temperatures. The Figure 2. FESEM micrographs of 共a兲 0.01, 共b兲 0.03, 共c兲 0.05 and 共d兲 0.07
observed orthorhombic phase of the present KNbO3 samples at mol concentrations of Nd3+-doped KNbO3 phosphors.
room temperature agrees with these reports. While increasing the
dopant 共Nd3+-ion兲 concentration from 1 to 7 mol %, when it reached
a certain limit 共greater than 3 mol %兲, the doping ability of the host
found to be the most intense peak. The emission mechanism can be
共KNbO3兲 becomes saturated and the redundant Nd3+ ions nullify the
explained based on the typical partial energy level diagram of Nd3+
precipitation effect, giving rise to a small amount of second phase
ions, as shown in the inset of Fig. 4. As can be observed, when the
formation. As can be seen in Fig. 1, the KNN01 and KNN03
Nd3+-doped KNbO3 phosphor is excited with 514.5 nm radiation of
samples are pure orthorhombic phases, while an additional phase is
an Ar+ laser, the Nd3+ ions in the ground state absorb the energy and
observed at the diffraction angle 2␪ of 27.80 and 29.45 共represented
by the ⴱ mark兲 at higher concentrations. This second phase can be are excited to the 4G9/2 level. After analyzing the Raman spectra,
Wen and co-workers19 reported that the maximum phonon energy in
attributed to NdNbO4 共JCPDS Card no. 22-1175兲. A similar type of
pure polycrystalline KNbO3 phosphor is 834 cm−1. Therefore, due
the EuNbO4 phase formation in Eu3+-doped KNbO3 phosphors was
to possible channels of cross relaxation and multiphonon relaxation,
also noticed by Fang and co-workers18 for Eu3+-ion concentrations
the nonradiative relaxations will take place and gradually decay
beyond 5 mol %. The influence of this second phase on the fluores-
cence properties of KNbO3:Nd3+ phosphors has been discussed in down to the 4F3/2 level. Then due to the sufficiently large energy gap
the present work. The 共111兲 peak is the most intense peak with a full between 4F3/2 and 4I15/2 levels 共approximately 5600 cm−1兲, radia-
width at half-maximum 共fwhm兲 共␤共2␪兲兲 varying from 0.27 to 0.33° tive emission 共R兲 will be predominated producing the NIR emis-
for different doping concentrations of Nd3+ ions. The crystallite size sions at 881, 1061, 1343, and 1800 nm as a result of 4F3/2 → 4IJ
共D兲 in the 共111兲 direction was calculated from the Debye–Scherrer transitions for J = 9/2, 11/2, 13/2, and 15/2, respectively. The
formula25,26
4
F3/2 → 4I15/2 emission at 1800 nm is not measured due to the lack
of experimental facility in that region. For more visual clarity, the
0.9␭ observed 4F3/2 → 4IJ 共J = 9/2, 11/2, and 13/2兲 emission peaks are
D= 关1兴 separately shown in Fig. 5. As can be seen in Fig. 5, the intensity of
␤共2␪兲 cos ␪
the emission peaks slightly increased from KNN01 to KNN03 and
where ␭ is the X-ray wavelength used, ␤共2␪兲 is the fwhm of the then decreased for higher concentrations, maybe due to the presence
diffraction peak, and ␪ is the Bragg angle. The crystallite sizes are of weak concentration quenching above 3 mol %. However, these
25 nm for the KNN01 and KNN03 samples 31 nm for the KNN05 slight changes in emission intensities cannot be completely attrib-
samples and 26 nm for the KNN07 samples. The observed crystallite uted to strong concentration quenching, as can be observed in vari-
sizes in the range of 25–31 nm in the present Nd3+-doped KNbO3 ous Nd3+-doped materials.27-29 A similar type of small changes in
phosphors are smaller than those in the range of 34–42 nm, as down-conversion emission intensities as a function of Nd3+-ion con-
reported for similar structured KNbO3 powders prepared by hydro- centration is also observed for Nd3+-doped LiNbO3 phosphors22 and
thermal synthesis.13 The crystallinity of the samples does not vary Ba2NaNb5O15 crystals.24 The fwhm was observed to decrease with
much with the variation in Nd3+-ion concentration, except the for- an increase in the concentration of Nd3+ ions as it was found to be
mation of an additional phase. The FESEM images of the samples 26.4, 26.2, 23.3, and 18.3 nm for KNN01, KNN03, KNN05, and
are shown in Fig. 2, which represent the surface microstructures of KNN07 samples, respectively. As can be clearly seen in Fig. 5, the
the KNbO3:Nd3+ phosphors under the present investigation. The emission peaks were split into various crystal-field 共CF兲 peaks, and
TEM images of the samples are also shown in Fig. 3. As can be seen the peak position of the 4F3/2 → 4I11/2 transition shifted from one
in Fig. 2 and 3, no obvious changes in morphology are observed CF peak at 1060.6 nm 共KNN01 and KNN03兲 to another one at
with increasing dopant concentration, and the particles are agglom- 1067.9 nm 共KNN05 and KNN07兲, with an increase in Nd3+-ion
erated with average particle sizes of less than 500 nm, which are concentrations. Similarly, a slight redshifting of emission peak po-
comparable to that of Eu3+-doped KNbO3 phosphors.18 sitions is observed in 4F3/2 → 4I9/2 and 4F3/2 → 4I13/2 transitions
The emission spectra for different concentrations of also. The emission peak positions 共␭p兲, effective linewidths 共⌬␭eff兲,
Nd3+-ion-doped KNbO3 phosphors were measured under a 514.5 and experimental branching ratios 关共␤R兲exp兴 of the observed emis-
nm excitation wavelength of an Ar+ laser and are shown in Fig. 4. sion transitions for different concentrations of Nd3+-ion-doped
As can be seen in Fig. 4, the spectrum consists of three emission KNbO3 phosphors, along with some reported Nd3+-doped systems,
bands near 881, 1061, and 1343 nm in the NIR spectral region, are presented in Table I. As can be seen in Table I, the redshifting of
which can be assigned to the 4F3/2 → 4I9/2, 4I11/2, and 4I13/2 transi- emission peak positions can be attributed to the increase in cova-
tions of Nd3+ ions, respectively. The emission peak at 1061 nm is lency arising from the reduction in Slater parameters 共Fk兲 and spin-
J66 Electrochemical and Solid-State Letters, 12 共7兲 J64-J68 共2009兲

Figure 3. TEM micrographs of 共a兲 0.01,

共b兲 0.03, 共c兲 0.05, and 共d兲 0.07 mol con-
centrations of Nd3+-doped KNbO3 phos-
phors.

orbit coupling parameter 共␨兲 due to changes in the overlap of the 1060 nm in the Nd3+-doped K3Li共2−x兲Nb共5+x兲O共15+2x兲 共KLN兲 single-
ligand orbitals with the 4f-electron wave function with an increase crystal fiber.24 The emission characteristics of Nd3+-doped LiNbO3
in Nd3+-ion concentration.30,31 The observed redshift can also be 共LNN兲 powders22 and channel waveguides33 and Nd3+-doped phos-
attributed to the formation of a second phase, which may make the phate glasses 共PKBAN兲 27 are also presented in Table I for compari-
Nd3+ ions occupy nonequivalent sites and experience different sym-
son. As can be observed from the 共␤R兲exp values, the relative con-
metries or different CF environments at higher concentrations.18 The
peak positions corresponding to the 4F3/2 → 4I11/2 transition at 1061 tributions of the 4F3/2 → 4IJ 共J = 9/2, 11/2, and 13/2兲 transitions in
共KNN01 and KNN03兲 and 1068 nm 共KNN05 and KNN07兲 in the the present KNN phosphors are comparable with that of earlier re-
present KNbO3:Nd3+ phosphor are comparable to those at 1064 nm ported Nd3+-doped systems.24,27,32 The variations in the emission
in the Nd3+-doped Li3Ba2Gd3共WO4兲8 共LBGWN兲 crystal32 and at characteristics of Nd3+ ions in different host materials might be at-

Figure 4. 共Color online兲 Emission spectra

of 共a兲 0.01, 共b兲 0.03, 共c兲 0.05, and 共d兲 0.07
mol concentrations of Nd3+-doped KNbO3
phosphors under 514.5 nm excitation. Par-
tial energy level diagram of
Nd3+-ion-doped phosphors representing
the emission mechanism is also shown as
the inset.
 Electrochemical and Solid-State Letters, 12 共7兲 J64-J68 共2009兲 J67

Figure 5. 共Color online兲 CF splitting pat-

terns of 4F3/2 → 4IJ 关J = 9/2 共i兲, 11/2 共ii兲,
and 13/2 共iii兲兴 transitions of Nd3+-doped
KNbO3 phosphors with 共a兲 0.01, 共b兲 0.03,
共c兲 0.05, and 共d兲 0.07 mol concentrations
of Nd3+ ions.

Table I. Emission peak position „␭p… (nm), effective linewidth „⌬␭eff…, (nm) and experimental branching ratio †„␤R…exp‡ of different transitions
of Nd3+-doped KNbO3 phosphors along with some reported Nd3+-doped systems.

Peak position 共␭p兲, 4F3/2→ Effective linewidth 共⌬␭eff兲, 4F3/2→

共nm兲 共nm兲 Experimental branching ratio 共␤R兲exp, 4F3/2→
4 4 4 4 4 4 4 4 4
Sample I9/2 I11/2 I13/2 I9/2 I11/2 I13/2 I9/2 I11/2 I13/2

KNN01 880.6 1060.6 1343.3 24.3 25.9 23.1 0.34 0.56 0.10
KNN03 880.6 1060.6 1343.0 26.6 28.3 25.7 0.30 0.59 0.11
KNN05 880.9 1067.9 1343.9 26.7 27.6 22.4 0.32 0.57 0.11
KNN07 881.2 1067.9 1343.9 32.4 24.9 22.5 0.32 0.57 0.11
LBGWN32 900 1064 1330 — — — 0.21 0.68 0.11
PKBAN27 892 1054 1325 38.0 25.5 41.9 0.28 0.59 0.12
KLN24 900 1060 1350 — — — 0.43 0.46 0.11
LNN22 890 1072 1340 — — — — — —
LNN33 900 1080 1300 — — — — — —

tributed to changes in the chemical and physical interactions in the 共␨兲 due to changes in the overlap of the ligand orbitals with the
nearest-neighbor coordination shell, where various factors such as 4f-electron wave function and the formation of a second phase with
bond lengths, bond angles, coordination number, and covalency de- an increase in Nd3+-ion concentration.
termine the energy, mixing, and splittings of the electronic states
involved in luminescence.34 Acknowledgments
This work was supported by the Korea Research Foundation
grant funded by the Korean Government 共grant no. KRF-2007-412-
Conclusions J00902兲.
Different concentrations of Nd3+-ion-doped KNbO3 phosphors Silla University assisted in meeting the publication costs of this article.
have been synthesized by the conventional solid-state reaction
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