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J o u rn a l o f R a d i a t i o n R e s e a r c h and A p p l i e d S c i e n c e s 8 ( 2 0 1 5 ) 3 9 9e4 0 3
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ScienceDirectJournal of Radiation Research and Applied
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Infrared spectroscopy and luminescence spectra ofYb3þ doped ZrO2 nanophosphor
Raunak Kumar Tamrakar a,*, Neha Tiwari b, Vikas Dubey a,Kanchan Upadhyay c
a Department of Applied Physics, Bhilai Institute of Technology (Seth Balkrishan Memorial), Near Bhilai House, Durg,
C.G. 491001, Indiab Department of Physics, Govt. Autonomous Science College, Jabalpur, Indiac Department of Chemistry, Shri Shanakayacharya Vidhyalay Hudco, 490006, India
a r t i c l e i n f o
Article history:
Received 15 December 2014
Received in revised form
21 February 2015
Accepted 27 February 2015
Available online 12 March 2015
Keywords:
ZrO2:Yb3þ
Infrared spectroscopy
Luminescence spectra
Combustion synthesis method
* Corresponding author. Tel.: þ91 982785011E-mail addresses: [email protected]
Peer review under responsibility of The Ehttp://dx.doi.org/10.1016/j.jrras.2015.02.0101687-8507/Copyright© 2015, The Egyptian Socopen access article under the CC BY-NC-ND l
a b s t r a c t
The present paper reports infrared spectroscopy and luminescence spectra of Yb3þ doped
ZrO2 nanophosphor. Sample was prepared by combustion synthesis method (CSM) for the
variable concentration of ytterbium. The low temperature synthesis method was suitable
for large scale production present method is an eco-friendly method as well as less time
taking method as compared to other methods. The synthesized samples were character-
ized by X-ray diffraction (XRD) technique; scanning electron microscopy (SEM), trans-
mission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FTIR)
technique. The crystal size was calculated by Scherer's formula. The particle size distri-
bution in prepared sample was determined by SEM and TEM study. The photo-
luminescence spectra was recorded under the 980 nm laser excitation with the variable
concentration of ytterbium. Here the PL intensity increases with increasing the concen-
tration of ytterbium. No concentration quenching were observed. The PL emission spectra
shows intense emission peaks at 987, 998 and 1021 nm all in infrared regions.
Copyright © 2015, The Egyptian Society of Radiation Sciences and Applications. Production
and hosting by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
1. Introduction
The research on inorganic luminescence materials having
high efficiency, good thermal and chemical stability has
revealed wide interests from last few decades. The emission
from rare earth ions doped luminescent materials in the op-
tical region of electromagnetic spectrum has been observed
through upconversion (UC) and downconversion (DC) pro-
cesses. Upconversion phosphors have a number of properties
3., raunakphysics@gmail.
gyptian Society of Radiat
iety of Radiation Sciencesicense (http://creativecom
that make them striking for photonics applications such as
display devices, lighting purposes, solar cells, biological ap-
plications, temperature and radiation sensors etc (Pandey and
Rai, 2012; Rai, 2007; Shalav, Richards, & Green, 2007; Singh,
Kumar, & Rai, 2009; Tiwari, Kuraria, & Tamrakar, 2014; Wang
and Liu, 2009).
In up-conversion and down conversion process, the low
phonon energy and high chemical stability are the critical
factors. Low phonon energy can prevent the non-radiative
energy loss with multi-phonon relaxation of rare earth
com (R.K. Tamrakar).
ion Sciences and Applications.
andApplications. Production and hosting by Elsevier B.V. This is anmons.org/licenses/by-nc-nd/4.0/).
J o u r n a l o f R a d i a t i o n R e s e a r c h and A p p l i e d S c i e n c e s 8 ( 2 0 1 5 ) 3 9 9e4 0 3400
dopants and enhance the energy transfer efficiency (Deng,
Wei, Wang, Chen, & Yin, 2011; Tamrakar, Bisen, & Brahme,
2014c; Tamrakar, Bisen & Brahme, 2015; Xia, Luo, Guan, &
Liao, 2012). Besides, the chemical stability is an essential
condition to the solar cells (Xia et al., 2012).
The special electronic configuration of Yb3þ makes the 4f
electrons less shielded than other ions of the lanthanide se-
ries, showing a higher tendency to interact with neighbouring
ions. Such an interaction is not restricted to different ions. It
has been reported that the YbeYb pair interaction produces
visible emission. That is, when there is neither an interme-
diate nor a final energy level (from the codopant) to be popu-
lated in order to emit in the visible.
In this paper, ZrO2:Yb3þ phosphor was prepared by a sim-
ple conventional combustion synthesis technique. The
structural properties of ZrO2:Yb3þ was characterized with X-
ray diffraction, Fourier transform infrared spectroscopy and
field emission scanning electron microscopy. Under excita-
tion with 980 nm laser, three NIR emission bands were
observed. The probable energy transfer mechanism is also
discussed.
Fig. 1 e XRD pattern of ZrO2:Yb3þ (4e16 mol%) phosphor.
2. Experimental
The starting reagents are high purity Zr(NO3)2, Yb(NO3)3$6H2O
and urea. Precursor materials were weighed in stoichiometric
ration and dissolved inminimumquantity of deionizedwater.
Then urea was added in this solution with molar ratio of urea
to nitrates based on total oxidizing and reducing valencies of
oxidizer and fuel (urea) according to concept used in propel-
lant chemistry. Finally the beaker containing solution was
placed into a preheated furnace maintained at 600 �C. Thematerial underwent rapid dehydration and foaming followed
by decomposition, generating combustible gases. These vol-
atile combustible gases ignite and burn with a flame yielding
voluminous solid. Urea was oxidized by nitrate ions and
served as a fuel for propellant reaction. The powders obtained
were then further calcined at 600 �C for 3 h to increase the
luminescence efficiency (Ekambaram & Patil, 1997; Tamrakar,
Bisen, & Brahme, 2014b; Tamrakar, Bisen, and Sahu, 2014;
Tamrakar, Bisen, Sahu, & Brahme, 2014b; Tamrakar, Bisen,
Upadhyay, & Brahme, 2014).
The XRD measurements were carried out using Bruker D8
Advance X-ray diffractometer. The X-rays were produced
using a sealed tube and the wavelength of X-ray was 0.154 nm
(Cu Ka). The X-rays were detected using a fast counting de-
tector based on Silicon strip technology (Bruker Lynx Eye de-
tector). (Dubey, Kaur, Agrawal, Suryanarayana, Murthy, 2013;
Dubey, Suryanarayana, Kaur, 2010; Dubey, Kaur, & Agrawal,
2013; Tamrakar, Bisen, Sahu and Bramhe, 2014a; Tamrakar,
Upadhyay, Bisen, 2014; Tamrakar, Bisen, Upadhyay and
Tiwari, 2014) Observation of particle morphology was inves-
tigated by FEGSEM (field emission gun scanning electron mi-
croscope) (JEOL JSM-6360). The photoluminescence (PL)
emission and excitation spectra were recorded at room tem-
perature by use of a Shimadzu RF-5301 PC spectro-
fluorophotometer (Tamrakar, Bisen, & Bramhe,et al 2014c;
Tamrakar, Bisen, & Upadhyay, 2015, Tamrakar, Kowar,
Uplop, & Robinson,et al 2014; Tamrakar, Tiwari, Kuraria,
Dubey, & Upadhyay, 2014).
3. Results and discussion
3.1. XRD results
The XRD pattern of the sample is shown in Fig. 1. The XRD
pattern recorded for variable concentration of Yb3þ (4 mol%e
16 mol%). The width of the peak increases as the size of the
particle decreases. The size of the particle has been computed
from the full width halfmaximum (FWHM) of the intense peak
using Scherer's formula (Dubey, Tiwari, Tamrakar, Rathore,
and Chitrakat, 2014; Kiryanov et al., 2003; Tamrakar, 2012,
2013; Tamrakar, Bisen, and Brahme, 2014a; Tamrakar et al.,
2013). Particle size of sample is found around 8e13 nm. For-
mula used for calculation is
D ¼ 0:9lb cos q
Here D is particle size
b is FWHM (full width half maximum)
l is the wavelength of X ray source
q is angle of diffraction
3.2. SEM analysis
The morphology of the prepared sample was determined by
using SEM analysis technique. Form SEM image of the sample it
canbeseen that thephosphorhasnano-sphere likemorphology
(Fig. 2). The diameter of the sample is about to 11 nm. The pre-
pared sample shows good phosphor particles have a spherical
shape. Indeed, phosphor particles with a spherical shape
minimize light scattering on their surfaces and therefore,
improve the efficiency of light, emission and the brightness of
such phosphor (Boukerika & Guerbous, 2014; Devaraju, Yin, &
Sato, 2009; Tamrakar, Bisen, Sahu, & Brahme, 2014a)
Fig. 2 e SEM micrographs of ZrO2:Yb3þ (4 mol%) phosphor.
Fig. 4 e PL emission spectra of ZrO2:Yb3þ (4e20 mol%)
phosphor.
J o u rn a l o f R a d i a t i o n R e s e a r c h and A p p l i e d S c i e n c e s 8 ( 2 0 1 5 ) 3 9 9e4 0 3 401
3.3. FTIR spectra
The phase formation and purity of the products are further
confirmed by FTIR spectroscopy, and results are shown in
Fig. 3. The strong transmittance peak 545 cm�1 is ascribed to
the stretching vibration of the ZreO bond. Like the PXRD re-
sults discussed earlier, FT-IR studies further confirms the
formation of pure ZrO2 product with no other major impu-
rities or secondary phases. Similarly the peak at 428 cm�1
ascribed the ZreO vibration (Sheetal et al., 2014; Wang et al,
2006).
3.4. Infrared PL spectra for luminescence study
The emission spectrum of ZrO2:Yb3þ phosphor at room tem-
perature was recorded. The emission spectra of phosphor
were found in near infrared region (NIR) (Fig. 4). The NIR
spectrum of ZrO2: Yb3þ phosphors have emission peaks at
1021 nm, 998 nm and 987 nm. The emission peak at 1021 nm is
the intense band whereas the other two emission peaks at
998 nm and 987 nm are comparatively smaller. The NIR
emission peaks are due to the transitions between the 2F7/2
Fig. 3 e FTIR spectra for ZrO2:Yb3þ (1e4 mol%) phosphor.
excited state and the 2F5/2 ground state for Yb3þ in ZrO2. The
two energy states splits into seven stark levels, 1 to 4 levels for
the ground 2F5/2 and 5-7 levels for 2F7/2 excited state. The
intense peak at 1021 nmattributed to the transition from stark
level 5/ 1, the peaks at lowerwavelength 998 nm and 987 nm
are due to transition 6 / 1 and 5 / 4 respectively (Fig 5).
The emission spectra was recorded as a function of Yb3þ
concentration from 4 to 20 mol% of Yb3þ concentration. No
emission was observed up to 4 mol% of Yb3þ in NIR region
above this concentration. The NIR emission due to Yb3þ ion
increases with increasing Yb3þ ion concentration. No con-
centration quenching observed for NIR emission upto 20mol%
Yb3þ ion concentration (Ermeneux et al 1997; Kiryanov et al.
2002; Montoya, Bausa, Schaudel, & Goldner, 2001; Nakazawa,
1979; Pandey et al., 2013; Tamrakar, Bisen & Bramhe, 2015;
Tamrakar, Bisen, Robinson, Sahu, & Brahme, 2014).
4. Conclusion
The ZrO2:Yb3þ phosphor has been prepared by using con-
ventional combustion synthesis method. The prepared
Fig. 5 e Energy level diagram for the NIR transitions.
J o u r n a l o f R a d i a t i o n R e s e a r c h and A p p l i e d S c i e n c e s 8 ( 2 0 1 5 ) 3 9 9e4 0 3402
phosphor was characterized by using powder XRD, SEM, FTIR
and TEM analysis method. For optical characterization of the
prepared phosphor emission spectra of the phosphors were
recorded. The emission spectra consists peaks in NIR region.
The NIR emission peaks are due to transition between 2F7/
2e2F5/2 states of Yb
3þ ion. The emission spectra were recorded
as a function of Yb3þ ion concentration. It was observed that
no concentration quenching were observed for with 5 mol%
concentrations of Yb3þ ion.
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