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Synthesis, characterization and photoluminescence properties of Ce3+-doped

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Article  in  Chemical Papers- Slovak Academy of Sciences · July 2013

DOI: 10.2478/s11696-013-0442-5

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 Chemical Papers
DOI: 10.2478/s11696-013-0442-5

ORIGINAL PAPER

Synthesis, characterization and photoluminescence properties

of Ce3+ -doped ZnO-nanophosphors

Sudheesh K. Shukla, Eric S. Agorku, Hemant Mittal, Ajay K. Mishra*

Department of Applied Chemistry, University of Johannesburg P.O. Box 17011, Doornfontein 2028, Johannesburg, South Africa

Received 19 October 2012; Revised 31 March 2013; Accepted 15 May 2013

The present study involves the synthesis of Ce3+ doped ZnO nanophosphors by the zinc nitrate
and cerium nitrate co-precipitation method. The synthesized nanophosphors were characterized
with respect to their crystal structure, crystal morphology, particle size and photoluminescence
(PL) properties using X-ray diffraction (XRD), scanning electron microscopy (SEM)/energy disper-
sive X-ray (EDX), transmission electron microscopy (TEM)/ Energy-dispersive X-ray spectroscopy
(EDS) and PL-spectroscopy respectively. XRD results revealed that ZnO nanophosphors are single
phase and cubic type structures. Further, PL spectra of ZnO:Ce3+ nanophosphors showed green
emission because of the charge transfer at single occupied oxygen vacancies with ZnO holes and red
emission due to the cerium ion transitions. Intensity and fine structure of the Ce3+ luminescence
and its temperature dependence are strongly influenced by the doping conditions. The formation of
ZnO:Ce3+ nanophosphors was confirmed by Fourier transform infrared (FTIR) and XRD spectra.

c 2013 Institute of Chemistry, Slovak Academy of Sciences

Keywords: nanophosphors, doping, co-precipitation, FTIR, photoluminescence

Introduction et al., 2010). Luminescent materials, i.e. nanophos-

Due to their unique and fascinating properties,
nanostructured materials have triggered tremendous
motivation among scientists to explore their applica-
tions. Alkaline earth oxides gathered a lot of atten-
tion in past decades because they are considered to
be excellent host materials. Nanoparticles are a new
group of advanced materials having different prop-
erties than bulk materials. These properties include
unique mechanical, chemical, physical, electrical, op-
tical and surface area, which in turn define them as
nanostructures. The most important characteristics of
the materials in the nano-size regime are their ability
to change their physical properties. During 1980s, a
considerable progress was achieved in the field of ma-
terial science to understand the size related proper-
ties in materials. When the size of the semiconductor
nanoparticles decreases, the energy gap (band gap) in-
creases and the optical spectrum is shifted towards the
short wavelength region (Murray et al., 1993; Kumar
phors, emit radiation when stimulated with fast elec-
trons, X-rays, ultraviolet photons or some other form
of radiation. In recent years, research has been boosted
by opto-electronic applications such as solid state
lighting, lasers, displays and optical storage media and
medical diagnostic applications like biological assays.
Various types of materials can be used for nanophos-
phor production. They have bixbyte type oxide hosts
with a cubic structure containing low symmetry sites
suitable for the incorporation of activators (rare earth
or transition metal ions) providing suitable emission
in the visible and near-infrared region.
Zinc oxide (ZnO), particularly, exhibits attractive
properties such as a wide direct band gap (3.37 eV)
(Hauschild et al., 2006; Klingshirn, 2007a; Jattaukul
et al., 2011), large excitation binding energy (60 meV),
low refractive index (1.9), resistance to high-energy
irradiation, stability to intense ultraviolet (UV) illu-
mination and low toxicity (Cruz-Vázquez et al., 2005;
Klingshirn, 2007b; Manam et al., 2009; Maciel et al.,

*Corresponding author, e-mail: amishra@uj.ac.za

ii S. K. Shukla et al./Chemical Papers
2010). ZnO nanoparticles are more versatile nanoma-
terials in biomedical applications due to their biocom-
patibility and high isoelectric point differences (∆IEP)
(Shukla et al., 2012). ZnO is a well suited semiconduc-
tor material with a variety of applications in the devel-
opment of UV optoelectronics because of its large ex-
citation binding energy and versatile band gap (Kling-
shirn et al., 2007). Moreover, ZnO is used in light
emitting diodes (LED), lasers, field emission devices
(FED), piezoelectric devices and chemical sensors due
of its remarkable optical, electrical and photoelectrical
properties (Zimmler et al., 2009).
Rare earth ions are widely used as activators in
different hosts due to their high fluorescence efficien-
cies and very narrow line fluorescence bands. Rare
earth doped nanophosphors are an attractive class of
materials with optical emission from the 4f–4f or 4f–
5d transition of rare earth ions. The emission wave-
length depends strongly on the surrounding crystal’s
field strength. Therefore, their emission can be tuned
by selecting an appropriate host lattice. Another at-
tractive property of rare earth doped nanophosphors
is that they are photo-stable and their surface can
be easily modified without altering their optical prop-
erties. This contribution introduces relatively simple
nanophosphors’ design and processing. These charac-
teristics make them suitable, for instance, for the use
in the development of immunoassays, time resolved
fluorescence imaging for quantitative histochemistry
and DNA detection. Photoluminescence of cerium
doped nanophosphors has been extensively studied be-
cause of the unusual interaction between the excited
states and the host lattice. Typically, rare-earth ions
emit from the well-shielded 4f orbitals and are there-
fore not significantly affected by the host lattice. How-
ever, Ce3+ is different because there is only one elec-
tron in the first shell of the 4f orbital (4f1 electronic
configuration), and its luminescence transition (4f–5d)
can occupy only low symmetry sites in the matrix, i.e.
ZnO, and appears as distinct bands in the excitation
spectra. Consequently, electrons are excited and emit
from the high-energy 5d–orbitals. The relative energy
of the 5d orbitals is highly dependent on the host lat-
tice.
In the present study, cerium doped zinc phos-
phors (ZCNP) was synthesized by the co-precipitation
method using Zn(NO3 )2 · 6H2 O and Ce(NO3 )3 · 6H2 O.
The synthesized ZCNP was characterized by Fourier
transform infrared (FT-IR) spectra, X-ray diffraction
(XRD), scanning electron microscopy (SEM), energy–
dispersive X-ray (EDX) and transmission electron mi-
croscopy (TEM). Moreover, the luminescent property
was also studied using a photoluminescence (PL) spec-
trophotometer.
Materials and methods
Starting materials for the synthesis of Ce3+ doped
ZnO nanophosphors and their source were: Zn(NO3 )2 ·
6H2 O (Aldrich, USA, 99.9 mass %), ethanol (Merck,
Germany, 99 mass %), Ce(NO3 )3 · 6H2 O (Aldrich,
USA, 99.9 mass %) and NaOH (Sigma–Aldrich, USA).
All supplementary chemicals were of analytical grade
and used without further purification. All working
standards and aqueous solutions were freshly prepared
with Millipore water (RO10TS) with the resistivity
levels of more than 18.2 MΩ cm at 25 ◦C.
Spectroscopic studies of Ce3+ doped ZnO nano-
phosphors were carried out with a Fourier transform
infrared spectrophotometer (PerkinElmer Spectrum
100) and a photoluminescence (PerkinElmer LS 45
fluorescence spectrometer with a Xe flash lamp) spec-
trometer. Crystal phase of the synthesized nanophos-
phors was determined by the X-ray powder diffraction
pattern taken on an X-ray diffractometer (Rigagu Ul-
tima IV) with CuKα (λ = 1.5405 Å) radiation. Par-
ticle size and morphology of the synthesized Ce3+
doped ZnO nanophosphors were determined on a scan-
ning electron microscope TESCAN (Vega 3 XMU)
and the samples were fixed on the sample holder us-
ing carbon coating. TEM analysis of the samples was
performed using a field emission electron microscope
(JEM-2100F). For TEM analysis, a drop of the syn-
thesized Ce3+ doped zinc nanophosphors solution was
placed on the TEM carbon coated copper grid and
the film on the TEM grid was allowed to dry for a few
minutes after removing the extra solution using the
blotting paper and heat.
Co-precipitation methods were used for the syn-
thesis of ZnO nanoparticles and Ce3+ doped ZnO
nanophosphors. Initially, an aqueous solution of 1 M
Zn(NO3 )2 and 1 M NaOH were prepared by dissolv-
ing each salt in double distilled water. The Zn(NO3 )2
solution (10 mL) was heated upto 60 ◦C under con-
stant stirring using a magnetic stirrer. Then, 1 M
NaOH (10 mL) was added dropwise. The mixture was
centrifuged and the suspension was discarded. The
precipitate was washed several times with absolute
ethanol and double distilled water. Ce3+ doped ZnO
was prepared in a similar manner; a calculated amount
of Ce(NO3 )3 added to Zn(NO3 )2 and allowed to mix
together homogeneously for 1 h under constant stir-
ring prior to the dropwise addition of NaOH. The pre-
cipitated slurry was kept in an oven at 100 ◦C for 12 h
to provide nanopowder Ce3+ doped ZnO nanophoh-
phorus; finally, the obtained products were annealed
at 600 ◦C.
Results and discussion
Fourier transform infrared spectroscopy
Fig. 1 shows the FTIR spectrum of ZnO and
Ce3+ doped ZnO powder after calcination at 600 ◦C.
The bulk information on the IR spectra of ZnO
lies between 500 cm−1 and 400 cm−1 . The peak at
 S. K. Shukla et al./Chemical Papers
Fig. 1. FTIR spectra of ZnO:Ce3+ nanophosphors, Zn (–),
Zn:Ce3+ (–).
Fig. 2. Photoluminescence spectra of ZnO:Ce3+ nanophos-
phors, Zn (–), Zn:Ce3+ (–).
530.93 cm−1 and 519.70 cm−1 were ascribed to ZnO
and Ce3+ doped ZnO respectively. The absorption
band at ≈ 3436 cm−1 was attributed to the O—H
stretching vibrations in both ZnO and Ce3+ doped
ZnO and originating from the surface OH groups. The
peak at 1613 cm−1 is due to the first overtone of the
fundamental stretching mode of the O—H bond. The
IR band between 519.70 cm−1 and 530.93 cm−1 can be
associated with oxygen deficiency and/or oxygen va-
cancy defect complex and ZnO (Kaschner et al., 2002).
Changes of the oxygen composition can be evaluated
also indirectly considering the intensity of the spec-
troscopic band at ≈ 500 cm−1 because this vibration
is caused only by the oxygen sublattice (Xiong et al.,
2006; Djelloul et al., 2010).
Photoluminescence analysis
Optical properties of the synthesized nanophos-
phors were analyzed by photoluminescence spec-
troscopy. PL spectra of ZnO:Ce3+ involves three
iii
Fig. 3. Energy level diagram showing the lowest energy ground
state component and first excited states of Ce3+ in
nanophosphors. The cubic crystal field splitting is indi-
cated by ∆ and the non-cubic splitting by δ (Wu et al.
(2007); Ye et al. (2010)).
Fig. 4. XRD pattern of nanocrystalline ZnO:Ce3+ nanophos-
phors, Zn (–), Zn:Ce3+ (–).
steps: i) excitation of the activator to a higher en-
ergy/excited state (10−11 s), ii) relaxation of the ac-
tivator ion to the lowest energy level of the excited
state (10−8 s) and iii) emission of a lower-energy pho-
ton as the activator ion returns from its excited state
to the ground state (10−9 s to 10−10 s) (Nalwa &
Rohwer, 2003). The Ce3+ ion is a well-known green-
emitting activator in commercial nanophosphors im-
proving their photoluminescence properties. Emis-
sions of Ce3+ are attributed to electronic transitions
from the lowest excited state to the ground state and
they strongly depend on their local environments in
the host lattice. The emission spectra of Ce3+ doped
ZnO nanoparticles were recorded by exciting the sam-
ple at the wavelength of 325 nm at room tempera-
ture (Fig. 2). The spectrum exhibits intense emission
peaks; one of them located at 392 nm (UV region)
corresponding to the near gap band electronic emis-
sion. A very broad emission spectrum was observed.
iv S. K. Shukla et al./Chemical Papers
Fig. 5. Scanning electron microscopy (SEM) of (A) Ce3+ undoped, (B) Ce3+ doped ZnO nanophosphor annealed at 600 ◦C; (C)
EDX curve of 3 atomic % Ce3+ doped ZnO nanophosphor.
The wide emission band is a result of the sum of emis-
sion peaks from 392 nm to 520 nm with a more in-
tense peak appearing at 440 nm. The intense peak at
440 nm is a result of the emission from Ce3+ doped
ZnO nanoparticles, which is due to the recombina-
tion of localized electrons at singly occupied oxygen
vacancies in deep trapped holes (van Dijken et al.,
2000; Li et al., 2003). The intense peak at 550 nm
can be assigned to the 5 D0 –7 F0 transition. The PL
bands at 392 nm and 440 nm are due to the cerium
ion transitions 2 D3/2 –2 F5/2 and 2 D3/2 –2 F7/2 , respec-
tively (Fig. 3, Patra and Ganguli (1992); Reisfeld et
al. (1999); Turos-Matysiak et al. (2006)).
XRD analysis
Crystal phase of the nanophosphor was determined
by the X-ray powder diffraction pattern with CuKα
(λ = 1.5405 Å) as shown in Fig. 4. Comparison of
the recorded XRD patterns with the standard JCPDS
card number 36-1451 shows that synthesized ZnO and
Ce3+ doped ZnO crystallites have wurtzite phase. No
other peaks were observed, which indicates the for-
mation of a pure wurtzite structure of ZnO and the
imbedding of Ce3+ ions in the host crystal lattice.
The results obtained show that the Ce3+ ions par-
tially replaced the Zn2+ ions in the host material.
Diffraction peaks at the 2θ values of 31.84◦, 34.50◦,
36.33◦, 47.65◦, 56.72◦, 63.01◦ and 68.11◦ correspond-
ing to (100), (002), (101), (102), (110), (103) and
(112) planes, respectively, were observed in the XRD
pattern of ZCNP. XRD data indicate that the oxi-
dized products are crystalline and single phase. The
mean particle size of ZCNP was calculated using the
Debye–Scherer’s equation (Kumaran & Gopalakrish-
nan, 2012):
Kλ
D= (1)
β cos(θ)
where D is the particle size, K is the constant (0.9), λ
is the wavelength of the X-ray radiation used (1.5405
Å), β is the full width at half maxima (FWHM) in the
radian of the (101) plane in the 2θ scale and θ is the
Bragg’s diffraction angle.
By fitting various peaks to this formula and tak-
ing the instrumental broadening into account, values
 S. K. Shukla et al./Chemical Papers v

Fig. 6. Typical transmission electron microscopy (TEM) images of Ce3+ undoped (A), Ce3+ doped (B), single Ce3+ doped ZnO
nanophosphor (size = 46 nm) annealed at 600 ◦C (C), and EDS curve of 3 atomic % Ce3+ doped ZnO nanophosphor (D).

in the range from 29.70 nm to 50.15 nm with the
mean value of 31.6 nm were obtained for Ce3+ doped
ZnO. Moreover, the observed slight shift of the ma-
jor diffraction peaks towards a lower diffraction angle
with dramatic decrease of the intensity along with the
3 % atomic doping with Ce3+ ions resulted in a shift of
the oxygen position in the ZnO lattice. The observed
broadening factor was assigned to the decrease of the
crystal size.
Scanning electron microscopy
Surface morphology of the synthesized Ce3+ doped
ZnO nanophosphor was examined by SEM as shown
in Figs. 5A and 5B, which reveal uniform distribution
of the synthesized nanophophors over the surface of
the ZCNP and good connectivity between the parti-
cles. There is a well observable morphology difference
between Ce3+ doped ZnO and ZnO alone. The EDX
spectra (Fig. 5C) confirmed the presence of Ce3+ in
the ZnO lattice; their atomic % being nearly equal to
their nominal stoichiometry within the experimental
error. According to the EDX data, 3 atomic % Ce3+
doping took place inside the zinc nanophosphors, sig-
nificantly influencing the red-luminescence behavior of
Ce3+ doped ZnO nanophophors.
Transmission electron microscopy
Typical TEM images of the Ce3+ doped ZnO
nanophosphors are shown in Figs. 6A and 6B. These
images confirm the existence of a bulk quantity of
spherically shaped cerium doped zinc nanophosphors
bunches. Each of these bunches is closely packed at
the nanometer scale (Moghaddam et al., 2009). The
average particle size in the present case varies in the
range of 30 nm to 51 nm with the mean value of
32 nm. There is a good correlation between the val-
ues obtained by mathematical calculation from an
XRD analysis and those obtained from TEM. The
EDS studies (Fig. 6C) also confirmed the presence of
3 atomic % of Ce3+ ions in the cerium doped ZnO
nanophosphors, significantly influencing their photo-
luminescence properties.
 vi S. K. Shukla et al./Chemical Papers
Conclusions
Ce3+ doped ZnO nanophosphors were obtained by
the co-precipitation method. FTIR studies clearly in-
dicated the presence of Ce3+ ions in cerium doped
ZnO nanophosphors. SEM and TEM analyses showed
the presence of the Ce3+ ion in the ZnO shell. The
particle size of Ce3+ doped ZnO nanophsophors varies
in the range of 30 nm to 51 nm with the mean aver-
age value of 32 nm. Moreover, there is a good corre-
lation between the values obtained by mathematical
calculation from the XRD (Debye–Scherer’s equation)
analysis and the results of the SEM and TEM studies.
XRD results also showed that synthesized ZnO:Ce3+
nanophosphor is crystalline with single phase. Photo-
luminescence spectra showed a wide band from the
Ce3+ doped ZnO nanophophors confirming the pres-
ence of green emission peaks at 392 nm and 440 nm.
The synthesized Ce3+ doped ZnO nanophosphor can
be explored for wider application in the field of pho-
tocatalysis and electrochemistry.
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