enhanced luminescence in camoo4: eu3+ red phosphor nanoparticles prepared by mechanochemically...
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Enhanced luminescence in CaMoO4:Eu3+ red phosphornanoparticles prepared by mechanochemically assisted solid statemeta-thesis reaction method
Anthuvan John Peter • I. B. Shameem Banu •
Jagannathan Thirumalai • Samuel Paul David
Received: 15 June 2013 / Accepted: 1 August 2013 / Published online: 15 August 2013
� Springer Science+Business Media New York 2013
Abstract For the first time, CaMoO4:xEu3? (x = 0.02,
0.04, 0.06, 0.08, 0.1) red phosphor nanoparticles were
synthesized using the simple mechanochemically assisted
solid state meta-thesis (SSM) reaction method and the
luminescence properties as a function of Eu3? ion con-
centration was investigated. The characteristics of the
phosphor materials were analyzed using X-ray diffraction,
fourier transform infrared spectroscopy, photolumines-
cence (PL) and diffuse reflectance spectroscopy. For
8 mol% of Eu3? concentration, the phosphor shows an
intensified excitation peak at 392 nm indicating a strong
absorption. The PL emission spectra of CaMoO4:Eu3?
phosphors showed an intense peak at 615 nm (red) which
corresponds to 5D0 ? 7F2 transition of Eu3?. The optimal
Eu3? concentration in CaMoO4 phosphors for enhanced
red emission occurs for 8 mol% and above this concen-
tration, the emission intensity decreases due to quenching
effect. The CIE colour coordinates of the Ca-
MoO4:0.08Eu3? red phosphor coincide very well with the
standard values of NTSC. The red emission intensity of the
SSM prepared CaMoO4:0.08Eu3? red phosphor is 4.7
times greater than that of the commercial Y2O2S:Eu3? red
phosphor and 1.6 times more than the same phosphor
prepared by the solid state reaction method.
1 Introduction
White light emitting diodes (LEDs), the next generation of
solid state lighting, have got much deliberate attention
recently due to their leverage over conventional light
sources such as, high efficiency, long life time, energy
saving, stability, environmental friendly, no pollutant and
have potential applications in many fields such as devices
like indicators, back lights, automobile head lights and
general illumination, etc. [1–5]. In general, conventional
white LEDs are assembled by combining a blue LED with
yellow emitting phosphor material, such as Y3Al5O12:Ce3?
[6] in which white light is generated when blue light from
the LED chip and yellow light from phosphor get blended.
However, such white light emitting diodes do not generate
warm white light due to deficiency of red emission [7].
This drawback is overcome by combining near UV-LED
chip (370–410 nm) with tricolor phosphors such as red,
green, blue phosphors to generate white light that can yield
a high colour rendering index. The UV light emitted by the
near UV-LED excites the tricolor phosphors giving white
light. The commercially available tricolor phosphors for
white LED applications are Y2O2S:Eu3? for red [8],
BaMgAl10O17:Eu2? for blue [9] and ZnS (Cu?, Al3?) for
green [10]. While comparing with blue and green phos-
phors, the thermal and chemical stability of the sulphide
based red phosphors is inadequate. They show poor
absorbance near UV region and their efficiency is also
approximately eight times lesser than blue and green
phosphors for white LED applications [11]. Therefore,
A. John Peter (&)
Department of Physics, St. Anne’s College of Engineering and
Technology, Panruti, Tamil Nadu, India
e-mail: [email protected]
I. B. Shameem Banu (&) � J. Thirumalai
Department of Physics, B. S. Abdur Rahman University,
Vandalur, Chennai, Tamil Nadu, India
e-mail: [email protected]
S. P. David
The College of Optics and Photonics, University of Central
Florida, Orlando, FL, USA
123
J Mater Sci: Mater Electron (2013) 24:4503–4509
DOI 10.1007/s10854-013-1433-6
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now-a-days, special attention is focused on discovering an
alternative novel red phosphor which is thermally and
chemically more stable and also shows better luminous
efficiency. To obtain a novel red emitting phosphor among
many rare earth ions, Eu3? is the best choice as an activator
ion because it can be effectively excited by near UV and
blue light and then emit stronger red fluorescence which is
ascribed to 5D0–7FJ (J = 0, 1, 2, 3) transitions [12–15].
In the recent years, an increasing attention is focused on
CaMoO4 as host matrix for luminescent ions due to their
good chemical and thermal stability and good lumines-
cence properties [16, 17]. CaMoO4 has scheelite structure
with a tetragonal unit cell (space group I41/a) and the
crystal structure has an inversion centre. Several works
have been reported on the luminescence properties of Ca-
MoO4:Eu3? red phosphors prepared by different methods.
Campos et al. and Longo et al. investigated the origin and
mechanisms behind photo luminescence properties of Ca-
MoO4 [18, 19]. Hu et al. [20] reported that CaMoO4:Eu3?,
red emitting phosphor can be excited by near UV light
(394 nm) to show strong red luminescence (616 nm) from
the Eu3? transition of 5D0–7F2 and thus considered to be a
good candidate for white LED application. Parchur and
Ningthoujam [21] described the luminescence properties of
Eu3? activated CaMoO4 phosphor and observed lattice
fringes by using FFT method. Chunlei et al. [22] studied
the luminescence properties of molybdate based phosphor
and they reported that scheelite host showed much stronger
UV absorption than wolframite host. There are several
routes to prepare calcium molybdate based LED phosphors
such as co-precipitation method [23], hydrothermal method
[24] and conventional solid state reaction (SSR) method.
SSR approach usually requires high temperature and con-
sumes a lot of power and time. The detailed literature
survey shows that so far no work has been reported on the
preparation of rare earth ion doped CaMoO4 phosphors by
mechanochemically assisted solid state meta-thesis (SSM)
route which can be performed at room temperature. The
solid state metathesis reaction method is an existing
method of synthesizing inorganic materials and has merits
compared to other traditional methods in terms of reaction
rate with little or no need for external energy. Using this
method, fine, chemically homogenous, pure and highly
crystalline phase phosphor material can be prepared in a
short time [25] at room temperature.
Based on these investigations, in this paper, the prepa-
ration of Eu3? doped CaMoO4 phosphors by mechano-
chemically assisted solid state meta-thesis (SSM) reaction
route is reported along with the observation of its red
emission enhancement for an optimal Eu3? doping con-
centration. The red emission intensity of the SSM prepared
sample has been compared with that of the same phosphor
prepared by SSR method and the commercially used
Y2O2S:Eu3? red phosphors to elucidate the advantage of
SSM method.
2 Experimental method
2.1 Preparation of phosphors
The red phosphors of CaMoO4:xEu3? (x = 0.02, 0.04,
0.06, 0.08, 0.10) were prepared by mechanochemically
assisted solid state meta-thesis route at room temperature
by using AR grade Na2MoO4�2H2O, CaCl2 and EuCl3(99.9 %) as the starting materials without any further
purification. The appropriate stoichiometric mixtures of
CaCl2, Na2MoO4�2H2O and EuCl3 were mixed and were
milled for a period of one hour in a planetary ball mill
Pulverisette 7 (FRITSCH). Milling was carried out in two
grinding vials of 15 ccm volume containing balls with
diameter of 12 mm. Both the container and balls were
made of tungsten carbide material. The number of milling
balls and the rotation speed of the planetary system of
milling device were kept constant. The resultant powder
was washed with distilled water to remove sodium chloride
and then dried at 80 �C for 3 h in a muffle furnace in air
and sieved.
CaCl2 þ Na2MoO4 � 2H2O! CaMoO4 þ NaCl
2.2 Characterization
X-ray powder diffraction (XRD) analysis was carried out
using Pan Analytical X’pert pro X-ray diffractometer with
Cu K-alpha radiation (k = 1.5406 A) at scanning rate of
0.02� per second. The XRD patterns were obtained in the
range of 0� B 2h B 70� and compared with the joint
commission on powder diffraction standards (JCPDS).
Fourier transform infrared spectroscopy (FTIR) measure-
ments were carried out in the wavenumber range of
400–4,000 cm-1 with a Nicolet 6700 FTIR equipped with
a deuterated triglycine sulfate detector. Photo luminescent
excitation and emission spectra were measured using a
Jobin Yuvon Flurolog 3-11 Spectrofluorometer at room
temperature with 450 W xenon lamp which was used as the
excitation source (200–700 nm). The phosphor powders
were slackly positioned on a solid stand and were excited
straight. The excitation and emission slit width were set to
2 nm. Optical absorption spectra were recorded using
Systronics-2101 UV–visible double beam spectrophotom-
eter. All spectroscopic measurements of the phosphors
were carried out at room temperature.
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3 Results and discussion
3.1 XRD analysis
The XRD profiles of CaMoO4:xEu3? (x = 0.02, 0.04, 0.06,
0.08, 0.10) are displayed in Fig. 1 with the corresponding
peaks indexed. Diffraction peaks of all the samples were
found to be similar without noticeable shift in the positions.
The XRD patterns of the doped samples match with the
diffraction pattern of the tetragonal scheelite structure of
CaMoO4 (JCPDS card no. 851267). The XRD pattern
signifies that the Eu3? ions have no obvious influence on
the structure of the host. No impurity peaks related to the
starting materials Na2MoO4�2H2O, CaCl2 and EuCl3 were
observed and this also suggests that doped Eu3? ions uni-
formly entered into the crystal lattice of CaMoO4. Since
the ionic radius of Eu3? (0.107 nm) is closer to Ca2?
(0.112 nm) [26], it is clear that Eu3? ion replaces the Ca2?
ion. The strong and sharp diffraction peaks indicate the
high crystallinity of the prepared samples [27] and hence it
clear that limited doping of Eu3? ions do not produce any
significant change in the crystal structure of the synthesized
phosphors [28]. The average crystallite size was deter-
mined according to the Scherrer’s equation. As described
in the literature [29]. Scherrer’s equation is D = 0.9 k/bcos h, where k is the X-ray wave length (0.15406 nm), b is
the full-width at half maximum (FWHM) of the diffraction
line and h is the diffraction angle. The average crystallite
size of the Eu doped CaMoO4 varies from 20 to 40 nm
which indicates that the particles are suitable for the
preparation of solid state lighting devices.
3.2 FTIR analysis
The FTIR spectra of CaMoO4:xEu3? (x = 0.02, 0.04, 0.06,
0.08, 0.1) phosphors are shown in Fig. 2. A very weak
absorption band lies around 430 cm-1 and it is associated
with the bending modes of vibration of Mo–O. A very
broad strong absorption band around 810 cm-1 is due to
anti-symmetric stretching vibrations of O–Mo–O in
MoO42- tetrahedron [21, 39]. The weak absorption band
around 3,400 cm-1 is due to O–H stretching vibration and
the bands around 1,630 cm-1 can be assigned to H–O–H
bending vibration of water absorbed from air [40].
3.3 Photoluminescence properties of CaMoO4:Eu3?
3.3.1 Excitation spectra analysis
Figure 3 shows the excitation spectra of CaMoO4:xEu3?
(x = 0.02, 0.04, 0.06, 0.08, 0.1) phosphors for monitoring
the 5D0–7F2 (kem = 615 nm) transitions of Eu3?. The
excitation spectrum consists of two parts: (1) a most
intense and broad excitation band in the range from 225 to
350 nm. (2) very sharp peaks with less intensity in the
range from 350 to 500 nm. The first region (200–350 nm)
is due to the overlapping of two charge transfer bands: (1)
Charge transfer transition from oxygen (O2- ligand) to
molybdenum (Mo6? ion) [ligand to metal charge transfer].
(2) Charge transfer transition from an oxygen 2p orbital to
an empty 4f orbital of europium [30–32]. Many weak sharp
lines in the second region between 350 and 500 nm cor-
respond to the typical Eu3? intra—4f transitions in the host
lattice. The strong absorptions at 392 and 462 nm were
attributed to the 7F0 ? 5L6 and 7F0 ? 5D2 transitions of
Eu3? which are in good agreement with the near-UV or
blue output wavelengths of GaN based LED chips [31].
Fig. 1 Powder XRD patterns of CaMoO4:xEu3? (x = 0.02, 0.04,
0.06, 0.08, 0.1)
Fig. 2 FTIR spectrum of CaMoO4:xEu3? (x = 0.02, 0.04, 0.06,
0.08, 0.1)
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3.3.2 Emission spectra analysis
Figure 4 shows the PL spectra of the CaMoO4:xEu3?
(x = 0.02, 0.04, 0.06, 0.08, 0.1) under 392 nm near-UV
excitation. The PL spectra of the synthesized samples are
similar with respect to the shape and peak positions and
differ in their peak intensities. The photoluminescence
emission spectra consists of sharp lines with wavelength
ranging from 530 to 710 nm, which are associated with the
5D0 ? 7FJ (J = 1, 2, 3, 4) transitions from the excited
Eu3? to the ground state. The main emission peak at
615 nm is strong which is due to the 5D0 ? 7F2 transitions
of Eu3? and the other transitions such as 5D0 ? 7F1,5D0 ? 7F3, and 5D0 ? 7F4 located in the range of
530–710 nm are weak [12]. The 5D0 ? 7F2 electric dipole
transition of Eu3? is highly sensitive to its surroundings
and occurs dominantly only when the Eu3? ion is in a non-
centrosymmetric site. Due to the lack of symmetry, the
4f orbitals mix with the opposite parity orbitals and thus the
electric dipole transition has occurred [34]. For this reason,
the intensity of 5D0 ? 7F2, was found to be much stronger
than those of 5D0 ? 7F1, which suggests that the Eu3? is
located in a distorted (or asymmetric) cation environment
and indicates that Eu 3? ions occupy the sites of Ca. Other
transitions from 5DJ (J = 1, 3, 4) are relatively weak,
which is advantageous when seeking to obtain high-quality
red light [35, 36].
3.3.3 Eu3? concentration effect
The doping concentration of Eu3? ions is one of the
important factors which influence the properties of lumi-
nescent materials. Hence, the optimum Eu3? doping con-
centration in CaMoO4:xEu3? (x = 0.02, 0.04, 0.06, 0.08,
0.1) phosphors for enhanced red emission was studied by
comparing the PL intensities obtained for various concen-
trations at the excitation wavelength of 392 and 462 nm.
Figure 5 shows the comparison of PL intensity ofFig. 3 PLE spectrum of CaMoO4:xEu3? (x = 0.02, 0.04, 0.06, 0.08,
0.1) phosphors monitored at 615 nm
Fig. 4 Photoluminescence
emission spectrum of
CaMoO4:xEu3? (x = 0.02,
0.04, 0.06, 0.08, 0.1) phosphors
under 392 nm excitation and the
inset shows PL spectra of
CaMoO4:0.08Eu3? phosphor
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Ca1-xMoO4:xEu3? (x = 0.02, 0.04, 0.06, 0.08, 0.1) (SSM)
phosphors excited by 392 and 462 nm as a function of
Eu3? concentration. For both the excitation wavelengths,
the PL intensity is observed to enhance with Eu3? con-
centration reaching a maximum at 0.8 % content which is
followed by a decrease with further increase in the con-
centration. This comparison reveals that the emission
intensity of phosphors excited at 392 nm (near UV) is
stronger as compared to that excited at 462 nm at almost
all the concentrations of Eu3?. Even though the maximum
red emission is obtained at 0.8 % for these two wave-
lengths, it is to be noted that the emission intensity for
392 nm (UV near) is much greater than that for 462 nm. It
signifies that they may be used as a potential red-emitting
phosphor in near-UV based White LEDs than blue GaN
based White LEDs. The optimum Eu3? content in CaMoO4
for the enhanced red emission is found to be 8 mol%.
The quenching of PL intensity for concentrations above
0.8 % may be due to the exchange interaction of energy
occurred between a number of excited Eu3? ions. For
europium activated phosphors, the quenching process is
attributed to the energy migration among the activators
(Eu3? ions) which brings excitation energy to the nearby
quenching centers (traps). These centers are typically
impurities or defects on the particle [37, 38].
3.3.4 Diffuse reflectance spectra and CIE analysis
It is known that the PLE spectrum is comparable to
absorption spectrum and so, the excitation band and peak
in the PLE spectra can be reasonably referred to one
absorption process (Fig. 3). To investigate the energy
absorption, the diffuse reflectance spectra (DRS) of Ca-
MoO4:xEu3? (x = 0.02, 0.08, 0.10) phosphors were mea-
sured and are shown in Fig. 6. The absorption band from
220 to 350 nm corresponds to overlapping of the (O–Mo)
ligand to metal CT in the MoO42- group and electron
transfer from oxygen (O2-) to europium (Eu3?). The
absorptions at 392 and 462 nm are ascribed to the 4f–
4f electron transitions of Eu3? ions, which is consistent
with the conclusion of the excitation spectrum analysis.
Figure 7 shows the CIE chromaticity diagram for the
emission spectra of CaMoO4:0.08Eu3? phosphor. The CIE
Fig. 5 Comparison of red emission intensities of CaMoO4:xEu3?
(x = 0.02, 0.04, 0.06, 0.08, 0.1) phosphors under 392 and 462 nm
excitation as a function of Eu3? concentration
Fig. 6 Diffuse reflectance spectra of CaMoO4:xEu3? (x = 0.02,
0.08, 0.1) phosphors
Fig. 7 CIE chromaticity diagram for CaMoO4:0.08Eu3? phosphor
(kex = 392 nm)
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chromaticity coordinates (x, y) of the CaMoO4:0.08 Eu3?
phosphor upon 392 nm excitation wavelength lie at
x = 0.678 and y = 0.322 which are very close to the
standard chromaticity coordinate values of NTSC
(x = 0.670, y = 0.330). Hence, the CIE diagram illustrates
that the obtained phosphor nanoparticles show red emis-
sions when excited by a single wavelength (kex = 392 nm)
and thus the obtained results confirm that the SSM pre-
pared CaMoO4:0.08Eu3? phosphor is a promising red
emitting components for near-UV InGaN-based white
LED.
3.3.5 Comparison of the photoluminescence
of CaMoO4:0.08Eu3? (SSM) with Y2O2S:Eu3?
and CaMoO4:Eu3? (SSR)
As the present work is focused for the purpose of red
phosphor application in WLED with near UV/blue GaN
based chips as excitation sources, the results of the PL
spectra of the present work (SSM) are compared with that
of (1) the PL spectra of CaMoO4:0.08Eu3? phosphor pre-
pared by SSR method and (2) the PL spectra of the con-
ventional red phosphor Y2O2S:Eu3? prepared by SSR
method. For this purpose, Y2O2S:Eu3? and CaMoO4:Eu3?
phosphors were prepared by SSR method and the lumi-
nescence properties were also studied. The red emission
spectra of these three red phosphors are presented in Fig. 8
which reveals that red emission intensity of Ca-
MoO4:0.08Eu3? (SSM) is about 4.7 times more than that of
commercially used Y2O2S:Eu3? red phosphor and 1.6
times more than that of CaMoO4:Eu3? (SSR) phosphor,
indicating that CaMoO4:0.08Eu3? phosphor prepared by
mechanochemically assisted solid state meta-thesis (SSM)
route at room temperature is a promising red phosphor for
WLEDs.
4 Conclusion
Well crystalline CaMoO4:Eu3? phosphor nano powders of
Scheelite-type have been successfully prepared by me-
chanochemically assisted solid state metathesis (SSM)
route at room temperature. The FT-IR spectra shown a very
intense and broad absorption band of the vibration in the
MoO42- tetrahedron. Upon 392 nm near UV excitation, the
CaMoO4:0.08Eu3? phosphor showed strong red emission
lines at 615 nm corresponding to forced electric dipole
transitions. The optimum doping concentration of Eu3?
content in CaMoO4 for the enhanced red emission is found
to be 8 mol%. The intensity of emission spectra of Ca-
MoO4:0.08Eu3? excited at 392 nm is remarkably stronger
than that of the same phosphor excited at 462 nm and this
suggests that CaMoO4:0.08Eu3? nanoparticles are suitable
red-emitting phosphor in near-UV based White LEDs than
blue GaN based White LEDs. The red emission intensity of
CaMoO4:0.08Eu3? reported in the present work is stronger
by a factor of about 4.7 times than that of the commercial
red emitting sulphide based phosphor, Y2O2S:Eu3? and
also it is about 1.6 times more as compared to that of
CaMoO4:Eu3? prepared by solid state reaction (SSR)
method. All these favourable properties indicate that SSM
prepared CaMoO4:0.08 Eu3? red phosphor is a promising
candidate for the phosphor converted white LEDs.
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