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Optical Band Gap and Photoluminescence Studies of Eu3+-doped Zinc Silicate

Derived from Waste Rice Husks

Article  in  Optik - International Journal for Light and Electron Optics · April 2019
DOI: 10.1016/j.ijleo.2019.01.061

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 Optik - International Journal for Light and Electron Optics 182 (2019) 486–495

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Original research article

Optical band gap and photoluminescence studies of Eu3+-doped

T
zinc silicate derived from waste rice husks
⁎
Rahayu Emilia Mohamed Khaidira, Yap Wing Fena,b, , Mohd Hafiz Mohd Zaidb,
Khamirul Amin Matoria,b, Nur Alia Sheh Omara, Muhammad Fahmi Anuarb,
Siti Aisyah Abdul Wahaba, Aisyah Zakiah Khirel Azmana
a
Institute of Advanced Technology, Universiti Putra Malaysia, 43400, UPM Serdang, Selangor, Malaysia
b
Department of Physics, Faculty of Science, Universiti Putra Malaysia, 43400, UPM Serdang, Selangor, Malaysia

A R T IC LE I N F O ABS TRA CT

Keywords: In this study, investigation on photoluminescence and optical properties of europium doped zinc
Zinc silicate silicate (Zn2SiO4:Eu3+) glass ceramics derived from white rice husk ash as potential silica source
Europium have been done. Undoped and 3 wt. % of europium doped zinc silicate were prepared by solid
Rice husk state method and sintered at 600–1000 °C for 2 h. XRD analysis revealed the phase formation of
Optical properties
amorphous, α or β-Zn2SiO4:Eu3+ phases of the glass and glass ceramic samples. FESEM results
Solid state
show the samples were irregular in shapes but well connected and formed large grain crystallites
as sintering temperatures increases. The optical band gap values for undoped samples are in-
creasing from 2.97 eV to 3.39 eV respectively. Meanwhile, the optical band gap values for 3 wt. %
Eu3+ doped samples decrease from 4.14 eV to 2.62 eV and increase again to 3.71 eV as sintering
temperature increases. PL analysis concludes that the red emission exhibited corresponding to
5
D0 → 7F2 electron configuration at 612 nm while excitation spectra was found at 400 nm at-
tributed to 7F0 → 5L6 transition. As conclusion, Eu3+ doped Zn2SiO4 glasses has potential as glass
host phosphor which can be used for optical devices such as plasma display panels (PDPs) and
cathode ray tubes.

1. Introduction

Over the past several years, rare earth oxides doped glass or glass ceramics has become one of the earliest discoveries and most
studied materials in a long history of research [1]. The initial interest in inorganic phosphor materials such as fluorides, phosphates,
borates, aluminates, silicates, and other oxides was primarily motivated by their properties of having low photon energies, chemically
stable and wide energy band gap when doped with rare earth ions [2]. Zinc silicate (Zn2SiO4) or also known as willemite has been
identified to be a great ideal host matrix phosphor for many rare earth and transition metal ions due to its excellent luminescence
properties in blue, green and red spectral regions which gives benefits in optical devices [3]. Hence, this inorganic phosphor materials
have been great interest in optical application devices such as lasers, laser cooling, optical communications devices, storage, displays
panels, upconverting optical devices and also electronic devices [4].
In recent years, Zn2SiO4 glass doped with rare earth ions has taken a great attention among researchers. Generally, glasses doped
with rare earth ions are better than transition metals due to its completely filled 4f shells, well shielded by 5s2 and 5p6 orbitals and

⁎
Corresponding author.
E-mail address: yapwingfen@gmail.com (Y.W. Fen).

https://doi.org/10.1016/j.ijleo.2019.01.061
Received 30 December 2018; Accepted 22 January 2019
0030-4026/ © 2019 Elsevier GmbH. All rights reserved.
R.E.M. Khaidir et al. Optik - International Journal for Light and Electron Optics 182 (2019) 486–495

their emission transitions yield sharp lines in the optical spectra providing phosphors with high luminescence efficiency [5]. Among
lanthanides, europium ions (Eu3+) is one of the most popular and useful rare earth ions due to its f-f transitions and luminescence
efficiencies in red spectral wavelength region mainly from 5D0 → 7F1,2 [6,7]. Other than doping, the structural, optical, mechanical,
thermal and electrical properties of the material could also be improved by controlling the applied heat treatment of the parent glass
[8]. Hence, this study focuses on the effects of different in sintering temperatures towards zinc silicate glass doped with europium
ions derived from waste rice husks.
Rice husk (RH) is one of the most abundant agro-industrial waste products for certain countries such as Malaysia and most
countries in south east area which takes up a lot of space and gives impact to environmental issues due to its burning process in order
to dispose the RH [9]. In this study, RH is used to replace commercial high purity silica to produce zinc silicate glass as it has been
proven to contain 95.60% of silicon dioxide [10]. Comparing to other sources such as soda lime silica (SLS), coconut husk ash (CHA)
and palm oil ash (POA), they contain about 69.50%, 91.76% and 45.50% respectively [11–13].
In this work, Zn2SiO4 based glass ceramics doped with Eu3+ derived from waste rice husks have been synthesized via solid state
method and its optical band gap and photoluminescence properties were investigated. Generally, there are various of methods that
can be used to produce Zn2SiO4 phosphor such as sol-gel method, spray pyrolysis method, hydrothermal method, co-precipitation
method and solid state method [14–18]. Among all these methods, solid state method is much simpler and could produce Zn2SiO4
glass ceramics in a large scale of production.

2. Experimental procedure

2.1. Starting materials and synthesis

RH was obtained from the local rice factory located at Tanjung Karang, Selangor, Malaysia. RH was soaked in a basin of water so
that all dirt and possible contaminants were submerged to the bottom. After being cleaned and dried in the oven for 12 h at 80 °C, the
dried RH were burned in the furnace at 1000 °C for 3 h and sieved to 45 μm powder size to obtain white rice husk ash (WRHA) which
proven to have high purity silica. Stoichiometric amount of starting materials, ZnO nanoparticles (US Research Nanomaterials, Inc.,
United State of America, 99+%, 10–30 nm), Eu2O3 (US Research Nanomaterials, Inc., United State of America, 99.99%, 5 μm) and
WRHA were mixed together using ball milling process to ensure the homogeneity of the powders. The composition of ZnO and WRHA
were fixed to 60:40 ratio respectively while Eu3+ concentration in the sample is kept constant at 0 wt.% and 3 wt.%. After mixing, the
powders were put to melting process at temperature of 1450 °C for 3 h and quench in a basin of tap water immediately for rapid
cooling process. The glass frits obtained from melt and quench process were crushed and sieved to 45 μm fine powder. Then, glass
powders were weighed into 1 g to prepare for pelletization process and sintered at different sintering temperature starting from 600
to 1000 °C. All pellets were crushed and grind to get uniform product and to ensure the characterization results are more accurate.

2.2. Characterization

The X-ray diffraction (XRD) patterns of the samples were confirmed by Phillips X’Pert High Pro PANanalytical Diffractometer
(XRD-6000) using Cu Kα radiation. The data measured over 2θ range between 20˚−80˚ were analyzed using X’Pert Highscore Plus
software and plotted using Origin Pro 8 software. The surface micrograph images of the pellet samples, which has been coated with a
thin layered of gold (Au) were observed using field emission scanning electron microscope (Nova NanoSEM 30 Series) under high
vacuum. All images have been taken under 10 000× magnification. The absorption spectra of the samples were determined by using
UV–vis-NIR spectrophotometer (Lambda 35, Perkin Elmer) in the wavelength range of 220–800 nm. From the absorption edges for all
samples, the optical band gap energy of the sample can be obtained. The emission and excitation spectra were performed at wa-
velength of 400 and 600 respectively, using Photoluminescence spectroscopy (Perkin Elmer LS 55). All measurements were carried
out at room temperature.

3. Results and discussion

3.1. X-Ray diffraction analysis

The amorphous and crystalline phase structure of prepared samples were analysed using XRD analysis and recorded in the range
of 20˚ - 80˚. The XRD patterns of undoped and 3 wt. % Eu3+ doped Zn2SiO4 sintered at various temperature from 600 to 1000 °C were
illustrated in Figs. 1 and 2 respectively. It was found that at room temperature up until 700 °C sintering temperature, the broad halo
peaks and presence of long range structural disorder were observed for both undoped and doped samples which indicates the
amorphous nature phase of the samples [19]. The graph obtained confirms the amorphous phase since there is no discrete or sharp
peaks observed from the XRD analysis of prepared samples [20]. After sintered at 800 °C, the undoped samples start to form crys-
talline phase structure which have been attributed to the well-developed major silicon dioxide, SiO2 phase (JCPDS 98-003-3025), β-
Zn2SiO4 phase (JCPDS 98-001-2169) and minor peak of zincite, ZnO phase (JCPDS 98-010-5282). This implies that the nucleation of
willemite phase starts after sintered at 750 °C and above. When sintering temperature was increased to 900 °C and 1000 °C, the β-
Zn2SiO4 phases were successfully transformed to a more stable state which is α-Zn2SiO4 (JCPDS 98-000-6041). It is also noticed that
the residual peaks of ZnO disappeared at these temperatures corresponding to successful decomposition of zinc nitrate [21]. The
maximum peaks obtained at 2θ = 25.21˚, 31.61˚ and 31.64˚ contributed to the graph of undoped Zn2SiO4 at sintering temperature

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Fig. 1. XRD pattern of undoped Zn2SiO4 sintered at various temperatures.

Fig. 2. XRD pattern of 3 wt. % Eu3+ doped Zn2SiO4 sintered at various temperatures.

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R.E.M. Khaidir et al. Optik - International Journal for Light and Electron Optics 182 (2019) 486–495

Fig. 3. FESEM images of undoped Zn2SiO4 sintered at (a) 27 °C (b) 600 °C (c) 700 °C (d) 800 °C (e) 900 °C (f) 1000 °C.

800 °C, 900 °C and 1000 °C respectively. From the graph, the intensity of the diffraction peaks increases and become sharper as
sintering temperature increases which indicates good crystallization occurs at high sintering temperature due to increase in diffusion
ions, hence increase in crystallite sizes and accelerate the crystal growth of the samples [22]. Diffusion ions occur when Zn and Si ions
are moving and diffusing in between the porosity of the samples thus forming α-Zn2SiO4 [23]. In Fig. 2, it was observed that the peak
intensities of 3 wt. % Eu3+ doped samples decrease when given heat treatment at high temperature. This is probably due to lattice
distortion in the structural system of the samples [24]. Eu3+ ions cause a strain in the system which leads to misalignment of the
lattice periodicity and decreases quality of crystal growth in the samples [25].

3.2. Field emission scanning electron microscopy (FESEM) analysis

FESEM analysis under 10 000× magnification was performed. Figs. 3 and 4 show the micrograph images of undoped and 3 wt. %
Eu3+ doped Zn2SiO4 sintered at different sintering temperature. It was observed that the distribution of particles are non-uniform and
irregular in shapes [26]. Starting from the unsintered samples, the surface morphology of the samples shows clear glassy surface with
no crystal growth appeared corresponding to the amorphous nature glass phase of the sample [27]. The grain sizes were also observed
to be small and high in porosity. This morphology observation explained why the unsintered samples were very fragile during
handling them. As sintering temperature was increased to 600 °C, the particles were starting to aggregate among each other and build

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R.E.M. Khaidir et al. Optik - International Journal for Light and Electron Optics 182 (2019) 486–495

Fig. 4. FESEM images of Zn2SiO4:3 wt. % Eu3+ sintered at (a) 27 °C (b) 600 °C (c) 700 °C (d) 800 °C (e) 900 °C (f) 1000 °C.

greater grains [28]. Next, the particles are observed to have good connectivity between grains as sintering temperatures were in-
creased up to 700 °C and 800 °C. The porosity between grains are also reducing and surface of the samples started to be melted-like
form [17]. Meanwhile, samples sintered at 900 °C becomes more densely packed with strong necking between the particles [3].
Lastly, when the samples were sintered at a very high temperature which is 1000 °C, the grains are closely packed showing less grain
boundaries among each other [29]. The grains appeared to be large in size thus making the surface morphologies of the 1000 °C
sintered samples to be smooth indicating the well crystallized ceramics had occurred as referred to XRD results [30]. In conclusion,
the sintering temperatures affect the surface and arrangement of the particles. Meanwhile, doping has given a small impact on the
surface morphologies of the samples [31]. Existence of Eu3+ dopant reduces the porosity of samples and the particles become more
densely packed thus forming a larger crystallites [32].

3.3. Absorbance analysis

The absorption spectra of undoped and 3 wt. % Eu3+ doped Zn2SiO4 glass ceramics sintered at various temperatures are presented
in Figs. 5 and 6. All these spectra were recorded in the wavelength range of 220–800 nm at room temperature. It was observed that all

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R.E.M. Khaidir et al. Optik - International Journal for Light and Electron Optics 182 (2019) 486–495

Fig. 5. Absorbance spectra of undoped Zn2SiO4 sintered at (a) 27 °C (b) 600 °C (c) 700 °C (d) 800 °C (e) 900 °C (f) 1000 °C.

Fig. 6. Absorbance spectra of Zn2SiO4:3 wt. % Eu3+ sintered at (a) 27 °C (b) 600 °C (c) 700 °C (d) 800 °C (e) 900 °C (f) 1000 °C.

absorption edges of the samples occurred in UV region between ˜250–400 nm for oth samples. Focusing on the undoped samples, the
absorbance edges are shifted to the left d found to be decreasing at lesser wavelength as sintering temperature increases. This explains
that the samples are highly crystalline as heat treatments are given up to 1000 °C as referring to XRD results [23]. Meanwhile, the
absorption edge of 3 wt. % Eu3+ doped samples are observed to be shifted to the right towards higher wavelength as sintering
temperature increases [33]. This occurrence happens due to the addition of dopant which enhance the absorption edges towards the
red shift that implies better glass crystallization in the samples [10].

3.4. Optical band gap

The optical band gaps of undoped and 3 wt. % Eu3+ doped Zn2SiO4 glass ceramics were calculated by using Mott and Davis
method. The relationship of absorption coefficient, α and photon energy (hv) can be describe as following equations [13];
(hv − Eopt ) n
a (v ) = A
hv (1)
By rearranging Eq. (1), the equation will be
1
(ahv ) = A (hv − Eopt )
n (2)
Where α is absorption coefficient, h is Planck’s constant, ν is frequency of vibration, A is proportional constant and Eopt is the optical
band gap energy. The exponent n varies according to the type of transitions where n = 1/2, 2, 3/2 or 3 which correspond to direct
allowed, indirect allowed, direct forbidden and indirect forbidden transitions respsectively. It was analysed that indirect allowed
transition where n = 2 has the best straight line for the samples compared to others. The Eopt values are calculated by extrapolating
the linear parts of (αhν)1/n versus hν (eV) curves to (αhν)1/n = 0.
Figs. 7 and 8 show the optical band gap measurement for undoped and 3 wt. % Eu3+ doped Zn2SiO4 sintered at various tem-
peratures based on plotted graph of (αhv)1/2 against hv, respectively. In this study, it was observed that as sintering temperature
increases from room temperature to 1000 °C, the optical band gap values of undoped sample are 2.97 eV, 3.19 eV, 3.11 eV, 3.09 eV,
3.22 eV and 3.39 eV respectively. Meanwhile, the optical band gap values for 3 wt. % Eu3+ doped samples are 4.14 eV, 3.55 eV,
3.35 eV, 2.62 eV, 2.88 eV and 3.71 eV respectively. The band gap values were observed to be fluctuate but increases at the highest
heat treatment (1000 °C) value. This explains the good crystallinity in the samples treated at higher sintering temperature due to the

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Fig. 7. Plot of (αhv)1/2 against hv of undoped Zn2SiO4 sintered at various temperatures.

Fig. 8. Plot of (αhv)1/2 against hv of Zn2SiO4:3 wt. % Eu3+ sintered at various temperatures.

vibration energy of the atoms that weakens the interatomic spacing between atoms thus, only small energy needed to break the bond
and led the electrons to freely move to conduction band which increases the band gap value [34]. By comparing the undoped and
doped samples, the optical band gap for doped samples are larger due to the enhancement of the samples’ crystallinities [35]. As the
doping concentration increases, the porosity of samples decrease and the particles become densely packed thus forming a larger
crystallites. Thereby, the band gap values increases as lesser defects and delocalization in the structural system of the samples [36].

3.5. Photoluminescence analysis

The excitation and emission spectra of the 3 wt. % Eu3+ doped Zn2SiO4 samples sintered at various temperatures were analysed
using photoluminescence spectroscopy to study the luminescence properties of Eu3+ doped phosphor as shown in Fig. 9(a) and (b)
respectively. The excitation spectra of samples recorded in the wavelength range of ˜350-550 nm were emitted under red light at
wavelength 600 nm. It revealed five distinguished characteristics peak centred at ˜400, 419, 457, 500 and 527 nm due to 4f-4f
transitions of Eu3+ ions configuration in the host lattice [37]. These five peaks are attributed to the 7F0 → 5L6, 7F0 → 5D3, 7F6 → 5D2,
7
F0 → 5D1 and 7F1 → 5D1, respectively [38]. The position of excitation bands observed corresponds to the luminescence properties of
Eu3+ being excited from ground state to various upper levels such as 5D or 5L [39]. As we can observed from the excitation spectra, at
room temperature, the excitation intensity was the highest while at temperature 1000 °C, the excitation intensity appeared to be the
lowest. The most intense band was 7F0 → 5L6 at the excitation peak near to ˜400 nm wavelength and this peak has been used to obtain
the red emission spectra from Eu3+ doping.
The emission spectra recorded in the wavelength range of ˜500-750 nm after being excited under blue light at wavelength 400 nm
was the most prominent excitation peak based on the absorption edge obtained previously. Results consist of five distinguished
characteristics peaks centred at ˜529 nm, 577 nm, 612 nm, 640 nm and 722 nm attributed to 5D1 → 7F1, 5D0 → 7F1, 5D0 → 7F2, 5D0 →
7
F3 and 5D0 → 7F4 corresponding to electronic transitions of Eu3+ ion, respectively [40]. Generally, the analysis of the spectral
features of 5D0 → 7F1 transition is due to the parity allowed magnetic dipole transition (ΔJ = 1) with orange-red emission to un-
derstand the symmetry crystal sites of doped Eu3+ ions and the intensities were observed to varies as sintering temperature increases
[41]. The red emission band exhibits at ˜612 nm attributed to 5D0 → 7F2 transition caused by the electric dipole transition (ΔJ = 2)
which the intensity depends on the local environment around Eu3+ ions in the host lattice [42]. The presence of forbidden spectra
5
D0 → 7F3 and 5D0 → 7F4 lower energy transitions are also visible [43].
As a conclusion, from Fig. 9(a) and (b), we can observed that the emission and excitation intensities of Eu3+ doped Zn2SiO4
fluctuated with subjects to sintering temperatures. The emission peaks attributed to 5D0 → 7F2 transition appeared highly as sintering

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Fig. 9. Photoluminescence analysis on (a) excitation (b) emission spectra of Zn2SiO4:3% wt.% Eu3+.

temperature increases up to 800 °C but dropped back to be single peak attributed to 5D0 → 7F1 transition when the sample was
sintered at 900 °C and 1000 °C. The increments are corresponding to the accumulation of Eu3+ ions in the host matrix leads to the
increasing of luminescence concentration in the samples [22]. Other than that, heat treatments also affect the transformation of Eu3+
ions to Eu2+ ions thus increase the Eu2+ emission intensity [44]. Meanwhile, the decrease in emission intensities are most probably
caused by the presence of high crystalline phase in the samples [45].

4. Conclusion

The synthetization of undoped and 3 wt. % Eu3+ doped Zn2SiO4 were successfully done via solid state method. All character-
ization analysis has been done to study the structural and optical studies of the samples by using XRD, FESEM, UV–vis and PL. Based
on XRD, different sintering temperatures affect the crystallinities of the samples as it formed high crystalline and sharp peaks with
increase in sintering temperature. The intensity of diffraction peaks dropped as Eu3+ dopant was introduced which is due to lattice
distortion where it reduce the crystal growth in the samples. FESEM shows the surface morphologies of the samples to be melted like
form as sintering temperature increases which indicates well crystalline ceramics had formed. As Zn2SiO4 was doped with Eu3+, the
porosity of the samples are reducing thus forming a densely packed grains. On the other hand, absorbance edges are found to be
shifting to the left and decreasing at lesser wavelength as sintering temperature increases. Meanwhile as dopant being added, ab-
sorbance edges are decreasing towards higher wavelength as sintering temperature increases. Optical band gap values for undoped
samples are increasing from 2.97 eV to 3.39 eV respectively. Meanwhile, the optical band gap values for 3 wt. % Eu3+ doped samples
are decreasing from 4.14 eV to 2.88 eV and then increase to 3.71 eV. PL analysis concludes that the red emission peak intensity found
was at 612 nm attributed to 5D0 → 7F2 electron configuration while excitation spectra was found at 400 nm attributed to 7F0 → 5L6

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transition.

Acknowledgements

Authors gratefully acknowledge all supports in terms of financial from Putra Grant (IPS) and Graduate Research Fellowship (GRF)
from Universiti Putra Malaysia (UPM). Lastly to Functional Devices Laboratory, Institute of Advanced Technology, UPM for lab
facilities support are also acknowledged.

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