Solid State Sciences 67 (2017) 8e12

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Solid State Sciences

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Investigations on structural and magnetic properties of Mn doped

Er2O3
Renu Tomar a, Parmod Kumar b, *, Ashish Kumar b, Ashok Kumar c, Pawan Kumar d,
R.P. Pant e, K. Asokan b, **
a
Department of Physics, BCAS, University of Delhi, Dwarka, New Delhi 110075, India
b
Materials Science Division, Inter University Accelerator Centre, New Delhi 110067, India
c
Department of Physics, D.C.R. University of Science & Technology, Murthal, Haryana 131039, India
d
Department of Physics, Kurukshetra University Kurukshetra, Haryana 136119, India
e
CSIR-National Physical Laboratory, Dr. K.S. Krishnan Road, New Delhi 110012, India

a r t i c l e i n f o a b s t r a c t

Article history: We report the structural, optical and magnetic properties of Mn doped Er2O3 samples. X-ray diffraction
Received 6 February 2017 study shows that dilute concentration of Mn in Er2O3 lattice leads to change in lattice parameter as well
Received in revised form as the crystallite sizes. The change in these parameters is attributed to difference in ionic radii of dopant
2 March 2017
and host. The changes in particle sizes and surface morphologies were confirmed by scanning electron
Accepted 4 March 2017
microscopy and their composition by energy dispersive X-ray measurements. Electron paramagnetic
Available online 9 March 2017
resonance (EPR) studies show that increase in Mn doping causes oxygen vacancies and hence
enhancement in magnetization. The intensities of Raman and photoluminescence spectra decreases with
Keywords:
Rare earth oxides (Er2O3)
Mn concentration inside the host lattice. Further, it is found that photoluminescence bands cover most of
Raman and photoluminescence the Raman band in the region of 200 cm
1e700 cm
1 when excited by 514 nm laser.
spectroscopy © 2017 Elsevier Masson SAS. All rights reserved.
Transition metal doping
EPR measurements

1. Introduction phases C (cubic, Fm-3m), B (monoclinic, C2/m) and H (hexagonal,

P63/mmc) [4,9e11]. It is well established that Er2O3 stabilizes in
Rare-earth (RE) sesquioxides have been widely used for many cubic phase (having space group la3ðTh7 Þ and unit-cell parameter
advanced technologies to reduce weight, energy consumption, ef- a ¼ 10.543 Å [12]) at ambient temperatures whereas monoclinic (B)
ficiency, speed durability and miniaturization applications due to phase crystallize at high temperatures [3,10]. In cubic crystal
their magnetic, luminescent, and electronic properties [1e4]. structure, unit cell of Er2O3 contains 16 formula units in which 32 Er
Among various RE oxides, erbium oxide (Er2O3) is a heavy oxide cations are distributed at two different sites (C2 symmetry with 24
and is most widely preferred as a key component of high- ions and C3i symmetry consisting of 8 ions) while 48 oxygen atoms
performance fiber optic communication systems [3]. It is also are present at 48 equipoints [10,11].
suitable for display purposes (such as display monitors) when its There are many reports in the literature on the uses of rare earth
nanoparticles are dispersed in glass or plastic and quite useful in oxides in telecommunication and bio-imaging applications [3e5],
surface modification for distribution into aqueous and non- but very limited reports on the magnetic properties of these ma-
aqueous media for bio-imaging [5]. Furthermore, the high dielec- terials. Wu et al. [13] have shown that Mn doping in Y2O3 samples
tric constant (>14) provides an alternative to use it as a gate lead to an enhancement in magnetization and it decreases after
dielectric material in metal oxide semiconductor devices with a annealing that is related with the change in oxygen vacancies. Arda
static dielectric constant [2,6e9]. Er2O3 exists in three different et al. [4] reported similar result in Co doped Er2O3 nanoparticles
wherein the intensity of EPR spectra increases with Co concentra-
tion. Based on these observations, it can be concluded that optical
and magnetic properties are closely associated with their structures
* Corresponding author. (i.e. change in oxygen vacancies) [9]. Therefore, the understanding
** Corresponding author.
of crystal structures and lattice vibrations of materials are of great
E-mail addresses: parmodphysics@gmail.com (P. Kumar), asokaniuac@gmail.
com (K. Asokan). interest. In view of this, the main objective of present work is to

http://dx.doi.org/10.1016/j.solidstatesciences.2017.03.003
1293-2558/© 2017 Elsevier Masson SAS. All rights reserved.
 R. Tomar et al. / Solid State Sciences 67 (2017) 8e12 9

understand the structural, optical and magnetic properties of pure The lattice parameter for pure Er2O3 sample is found to be ~10.53 Å.
and Mn doped Er2O3. In these systems, it has been found that there A visual inspection over XRD pattern depicts that most intense peak
is small change in the structural and morphological properties (222) shifts towards higher angle side up to 3% Mn doping. The
depending upon the preparation methods and dopant concentra- shifting in (222) peak towards higher angle results in decrease in
tions, but significant changes in the magnetic properties. Therefore, lattice parameter (as shown in Table 1). The reduction in lattice
the main focus of present work is to understand the effect of dilute parameter with Mn composition is attributed to smaller ionic radii
concentration of Mn (up to 5%) on the various physical properties of Mn ions (0.67 Å) as compared to that of rare earth Er3þ ions
with special emphasis on the magnetic properties of Er2O3. (0.88 Å). However, further increase in Mn doping (i.e. for 5%) causes
the shift towards lower angle side. The opposite trend for higher
2. Experimental details doping concentration (for 5%) might be associated to the solid
solubility limit of Mn ions into Er2O3 lattice. Similar kind of varia-
Pure and Mn (1%, 2%, 3% and 5%) doped Er2O3 samples have been tion (i.e. random distribution of dopants after certain concentra-
synthesized via solid state reaction method using MnO2 (99.99%) tion) has also been discussed elsewhere for Mg doped ZnO, Y doped
and Er2O3 (99.99%) as initial starting materials. The appropriate ZnO, Mn doped CeO2 and C implanted ZnO samples [14e16].
amount of precursors were mixed, ground for 2 h using mortar and Furthermore, the average crystallite size of Mn doped Er2O3 sam-
pestle and then calcined at 600  C for 5 h to obtain the desired ples was determined using Debye-Scherer’s formula (D ¼ 0.89l/
phase. After calcination, the powder was again grounded, pelletized bcosq) [17], where D is crystallite size, b is full width at half maxima,
and then sintered at 800  C for 6 h to densify the pellets in order to q is Bragg's angle and l is wavelength of CuKa. The crystallite size for
achieve homogeneity. The synthesized samples were then charac- pure Er2O3 sample is ~34 nm. However, no regular variation in size
terized for their structural, optical and magnetic properties using is detected with doping due to dilute concentration of Mn ions in
different experimental techniques. The crystal structure of Mn host lattice (Table 1).
doped Er2O3 samples were confirmed using Rigaku X-ray diffrac-
tometer having CuKa source of wavelength 1.54 Å. The change in 3.2. Scanning electron microscopy (SEM) & energy-dispersive X-ray
the morphology, particle size and composition was estimated from spectroscopy (EDX)
HitachieTM 3000 scanning electron microscopy (SEM) along with
energy dispersive X-ray spectroscopy (EDX). Raman spectroscopy SEM images of pure, 2%, 3% and 5% Mn doped Er2O3 samples
measurements were performed with Arþ ion laser beam having were recorded for morphological studies and are shown in Fig. 2.
wavelength of 514 nm and 50 mW power (Renishaw). The optical SEM images confirm the formation of well-defined particles for all
properties were studied with Renishaw photoluminescence spec- the samples. The particle size for pure Er2O3 sample is found to be
trometer using two different lasers having wavelengths 325 nm ~106.24 nm. The doping of Mn ions in the host lattice changes the
and 514 nm respectively. The electron paramagnetic resonance morphology as well as the particles size. It has been found that the
(EPR) measurements were carried out on X-band EPR spectrometer shape of well-defined pure Er2O3 sample changes with the addition
(Make: Bruker Biospin, Model: A300). The weighed samples were of Mn ions. The Mn doped samples are much denser compared to
taken in transition metal ions free quartz capillary tubes and pure Er2O3 sample. The particle size reduces continuously with the
aligned at the centre of rectangular cavity. The spectra were addition of Mn ions due to lower ionic radii of Mn ions (0.67 Å) than
recorded at 9.56 GHz microwave frequency in 4000 ± 4000G scan Er ions (0.88 Å) [14]. The variation in the particle size is in accor-
range. DPPH has been used as a standard reference material for the dance with the results obtained from XRD. It is worth to mention
estimation of g-value, spin concentration and EPR parameters. here that there is not much change in the crystal structure as well
as in morphological properties. However, there is significant effect
3. Results and discussion on the magnetic properties when dilute concentration of magnetic
ions is added in the host lattice. This is consistent with many re-
3.1. X-ray diffraction ports in the literature especially on dilute magnetic ions doped
semiconductors like ZnO, TiO2, CeO2, etc [4,16e19].
XRD patterns of pure and Mn doped Er2O3 samples are shown in EDX measurements were further carried out to estimate the
Fig. 1. All the diffraction peaks observed correspond to single phase doping concentration of Mn ions in the host lattice. Fig. 3 shows the
cubic structure of Er2O3 (referred to the JCPDS Card No. 77e0777). EDX study of pure and Mn doped samples and suggest an increase
in the Mn content with the doping concentration.

3.3. EPR spectra

EPR spectrum is very sensitive and powerful resonance tech-

nique based on microwave absorption of unpaired electron spins in
presence of an external magnetic field to explore electronic struc-
tures, lattice defects, color centers, and magnetic phases (para-
magnetic and/or ferromagnetic) present in a material [20e22]. It
has been found that very small concentration of Mn2þ ions in
diamagnetic materials show electron-nuclear hyperfine interaction
features in EPR spectrum. While at higher Mn2þ concentrations, a
single broad line due to exchange interactions has been observed.
The exchange interaction between Mn2þ and Mn3þ oxidation states
gives a single broad line at room temperature. In this work, EPR
technique has been used to investigate the incorporation of Mn
dopant in Er2O3 host lattice with increasing Mn concentration from
1% to 5%.
Fig. 1. XRD pattern of pure and Mn doped Er2O3 samples. EPR spectra of different Mn doped Er2O3 compositions recorded
10 R. Tomar et al. / Solid State Sciences 67 (2017) 8e12

Table 1
Various parameters for Mn doped Er2O3 samples observed from XRD, SEM and EPR measurements.

Composition Lattice parameter (Å) Crystallite Size Particle Size(nm) DHPP g-value NS  1012 Relaxation Time  10
6
(nm) (Gauss) (spin/g) (ts)

Pure Er2O3 10.53 36.3 106.2 e e e e

1% Mn 10.52 37.5 98.7 316.3 2.19 4.89 269.48
2% Mn 10.50 34.5 96.2 665.6 2.06 3.43 136.36
3% Mn 10.49 31.6 91.7 731.5 2.04 2.82 289.98
5% Mn 10.52 34.9 88.4 303.1 2.15 3.56 128.23

at ambient temperature are presented in Fig. 4 and summarized the reduction in intensity is due to fact that the rate of change of
values of EPR parameters in Table 1. DPPH was used as a standard concentration is low. Mn doping in Er2O3 lattice substitutes Er3þ
reference material for magnetic field marker and evaluation of site and have a strong tendency to attract electrons [23]. The
paramagnetic spin concentration. EPR spectra show a narrow electron trapped on Mn2þ ion causes a transition between 3d and
resonance line with g-value ~1.98 and broad signal with g-value in Er 4f orbitals start and causesresults in the appearance of EPR
the range from 2.04 to 2.19. EPR spectra of Er2O3 shows W-shaped signal. To compensate the charge imbalance, the oxygen vacancy is
signal characteristics of RE materials pertaining to Er3þ para- formed [24]. The oxygen vacancy occurs in three different charge
magnetic ions with ½ spin. Incorporation of low doping concen- states: (i) neutral; (ii) singly ionized and (iii) doubly ionized [25,26].
tration (1% Mn doping) in host lattice results in the significant The g-values for signal originating from shallow donors and singly
enhancement in peak intensity and thereafter (for 2%, 3% and 5% ionized oxygen vacancies or unpaired electron trapped on an oxy-
Mn doping) small reduction in intensity is detected. This small gen vacancy sites are at 1.96 and 1.99 respectively. Based on the
analysis, the EPR spectra show the presence of Mn2þ and an un-
paired electron trapped in Mn3þ (a narrow line). A signal at g-value
of 1.98 (a broad line) has been assigned to an unpaired electron
trapped on an oxygen vacancy site or singly ionized oxygen va-
cancy, respectively. The g-value of these signals reduces from 2.19
to 2.04 with increasing Mn2þ concentration from 1% to 3% and it
increases to 2.15 for 5% Mn doped sample. The spin concentration
(NS) decreases from 4.89  1012 to 2.82  1012 with increasing Mn
ion concentration from 1% to 3% and then it increases to 3.56  1012
for Mn 5% doped sample. It means that increasing Mn concentra-
tions from 1% to 5% leads to decrease in total number of spins
contributing to this line. This indicates a decrease in Mn2þ ions
concentrations or unpaired electron trapped in Mn3þ, while the
total number of spin contributing to broad line increased, sug-
gesting an increase in oxygen vacancy concentration with doping.
It is observed that relaxation time (ts) decreases with an in-
crease in Mn2þ ion content from 1% to 2%. The variation in relax-
ation time is not systematic. The change in spinespin relaxation
time is attributed to the decrease in electron motion in Mn 2%
sample and weakening of superexchange interaction in lattice.
While in Mn 3% sample, the relaxation time is improved due to
enhancement of superexchange interaction among cations through
Fig. 2. SEM images of pure and Mn doped Er2O3 samples. oxygen ions. The relaxation time further decreases from
289.98  10
6 to 128.23  10
6 when Mn ion concentration in-
creases from 3% to 5%.
At doping concentration of 1 at%, line shape of the sample is
dominated by Mn2þ ions or an unpaired electron trapped in Mn3þ.

Fig. 3. EDX measurements for pure and Mn doped Er2O3 (2%, 3% and 5%) samples
where inset of each figure shows the variation of element with its wt %. Fig. 4. EPR spectra of pure and Mn doped Er2O3 samples.
 R. Tomar et al. / Solid State Sciences 67 (2017) 8e12 11

value of line width (DHPP) and minimum g-values has been ach-
ieved by doping Er2O3 with 3% Mn.

3.4. Raman spectroscopy

Raman spectroscopy provides complimentary information for

detailed crystal structure especially phase of the materials. As
mentioned above, XRD measurement confirms that Er2O3 crystal-
lizes in the cubic structure with space group la3ðTh7 Þ. According to
crystallography, various optical modes associated with its vibra-
tions at Gepoint are expressed as

G ¼ 5Au þ 5Eu þ 17Tu þ 4Ag þ 4Ag þ 14Tg :

Here, Au and Eu modes are Raman inactive whereas Tu modes are

infrared active. Apart from these, Ag and Tg symmetries are found to
Fig. 5. Raman spectra of pure and Mn doped Er2O3 samples excited by 514 nm laser.
be Raman active. Fig. 5 shows Raman spectra for all samples in the
range of 200e700 cm
1. Several peaks were observed in pure and
doped samples at ~293, 308, 337, 367, 381, 405, 439, 482, 558 and
At this doping concentration, the signal at g-value of 1.98 was not 595 cm
1. The spectral assignment of observed peaks for all the
observed. This may be due to the very low concentrations of oxygen samples is given in Table 2. The major peaks at ~381 cm
1 and
vacancy which are below the detection limit of EPR instrument. As ~439 cm
1 in the samples have been assigned to Tg mode whereas
the doping concentration is increased, the narrow line shifts to- peak observed at ~337 cm
1 corresponds to Eg mode of Er2O3.
wards higher applied magnetic field, and the line width increases Strong Raman intensity measured for Tg mode indicates a large
from 316.3 G to 731.5 G up to 3% samples and then reduces to polarizability change during the vibration. Therefore this band is
303.1 G in 5% Mn2þ doped sample. The strong dipolar-dipolar expected to be more sensitive towards changes in chemical
interaction superexchange interactions among cations through bonding in the series. Tucker et al. [27] have also observed similar
oxygen ions may be the possible reason for change in EPR line intense peak for this mode in Raman spectra of Ce type rare earth
width. From EPR results, it has been observed that the maximum sesquioxides like Eu2O3, Dy2O3 and Tm2O3 in ambient conditions.

Table 2
Raman peaks of Er2O3 (where band intensity: S-strong, Vs-very strong, m-medium, W-weak, Vw-very weak).

S. No. Peak positions Intensity Refs. [9] Refs. [28,29] Raman active modes (assigned)

1 293 298
2 308 Vw 316 Eg þ Tg
3 337 S 336 338 Eg
4 367 Vw 359 359
5 381 Vs 381 381 Tg
6 405 W 404 405 Tg
7 439 W 436 Tg
8 482 S 480 480 Tg
9 558 W 580 580 Tg
10 595 S 600 598 Tg

Fig. 6. Photoluminescence spectra of pure and Mn doped Er2O3 excited by 514 nm and 325 nm laser.
12 R. Tomar et al. / Solid State Sciences 67 (2017) 8e12

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