IOSR Journal of Applied Physics (IOSR -JAP) [601691]

IOSR Journal of Applied Physics (IOSR -JAP)
e-ISSN: 2278 -4861.Volume 10, Issue 5 Ver. I ( Sep. – Oct. 2018), 47-56
www.iosrjournals.org

DOI: 10.9790/4861 -100501 4756 www.iosrjournals.org 47 | Page Tuning the optical properties of Fe2O3 doped ZnO / Polystyrene
composite films H.

Abomostafa*a, G. M. El komyb, S.A. Gadc, M.M. Selimd
aFaculty of Science, Physics dept. , Menoufia University, Egypt
b Electron Microscope and Thin films Dept., Physics Research Division, National Research Centre, El -Bohoos
str., 12622, Dokki, Giza, Egypt
c Solid State Physics Dept., Physics Research Division National Research Centre, El -Bohoos str., 12622, Dokki,
Giza, Egypt
dPhysical Chemistry dept., National Research Centre, El -Bohoos str., 12622, Dokki, Giza, Egypt
Corresponding Author: Abomostafa*a

Abstract : The effect of addition of Fe2O3 doped ZnO nanoparticles on some optical properties of polystyrene
has been studied. Fe2O3 doped ZnO nanoparticles was prepared by combustion method. Polymeric films based
on polystyrene (PS) filled with different weight percentage (5, 7.5, 10, 12.5) were prepared by the casting
method. The morphology of the prepared filler of Fe 2O3 doped ZnO n anoparticles were verified by high –
resolution transmission electron microscope (HRTEM). Structures of the prepared films were examined by x –
ray diffraction (XRD), where the recorded pattern reveals the existence of wurtzite phase of hexagonal structure
for ZnO nanoparticles doped with Fe 2O3. The absorption, transmission and diffuse reflectance spectra were
recorded in the visible range. The absorption coefficient, optical band gap, extinction coefficient, and refractive
index of the casted films were calc ulated. The results showed a sharp decrease in the band gap from 4.54 to
2.82 eV with increasing the percentage ratio of Fe 2O3 doped ZnO nanoparticles in PS matrix.
Keywords : Fe2O3 doped ZnO nanoparticles, polystyrene, Inorganic/organic composite films, opt ical properties .
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Date of Submission: 03 -09-2018 Date of acceptance: 18 -09-2018
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I. Introduction
Inorganic/ organic composite material plays an important role in creating extensive usages in many
areas. It is used in a wide search for high permittivity materials that have extensive variety ofof technologically
important applications for example, micro electronic, embedded passive and electrostrictive devices. Polymer
composites are used as electrically conductive adhesives and circuit elements in microelectronics and have been
reported to possess anticorrosive behavior as metal components coatings [1].P olymer composites are utilized as
electrically conductive glues and circuit components in microelectronics and have been accounted for to have
anticorrosive conduct as metal parts coatingsOne of the most interesting polymers is the polystyrene; it has
excellent physical and chemical properties. Polystyrene is an amorphous polymer with high transparency, ease
of process and it is very important in many industrial applications [2, 3].It was reported that a conductive or
semiconductive composite is formed by d ispersion of sufficient quantity of metallic particle [4]. The dispersion
of metals nanoparticles in the polymer matrix could commonly add unique physical properties to the associated
matrixes such as responsiveness to mechanical, optical, thermal, magne tic, electric stimulation, etc to produce
very useful nanocomposites [5, 6]. Also metals – polymer matrix is relatively not costly in the point of view of
the processing techniques and manufacturing materials as compared to the expensive materials widely u sed in
semiconductor processing industry [7]. Zinc oxide, ZnO is one of many inorganic materials. It has direct band
gap (Eg = 3.27 eV) [8, 9] which is considered a promising candidate for optical and optoelectronic applications
in nano -scale devices. [10, 11]. In spite of these preferences of ZnO, its functional applications were constrained
by some acquired disadvantages, for example the requirement of UV light activation, the low quantum
efficiency, and the serious photo -corrosion [12]. To overcome these problems, ZnO matrix composite
semiconductors containing some other reinforcing particles that have novel and advanced properties.
Especially, because of the easy availability, nontoxic nature, biological and chemical stability, nanostructure
semiconducto r metal oxides such as TiO2, SnO2, CuO, WO3 and Fe2O3 have become promising photocatalysts
in environmental improvement [13 –21]. Among the metal oxides, hematite (α -Fe2O3) is the most
thermodynamically -stable phase of iron oxide under ambient conditions wi th low cost, high resistance to photo –
corrosion and environment -friendly features. It can be driven by visible light up to 600 nm due to the narrow
band gap of 2.2 eV, and has been confirmed to be an important member of visible -light-responsive
semiconduct or photocatalysts [22 -26]. Different methods have been used to synthesize various metal -polymer

Tuning the optical properties of Fe2O3 doped ZnO / Polystyrene composite films H. ..
DOI: 10.9790/4861 -100501 4756 www.iosrjournals.org 48 | Page composites E.g. (i) Direct mixing of nanoparticles in the polymer [27] (ii) Sol -gel methods [28] (iii) in -situ
techniques [29] and (iv) deposition method [30]. Many types of polymer composites have been studied by
introduction of conductive filler such as, silver (Ag), nickel (Ni), Aluminum (Al), Ni/Co coated CNT in
polystyrene composite and carbon nanotube (CNT) [31 -35].

In this work,
 We successfully synthesiz ed nanoparticles of Fe 2O3 doped ZnO by combustionand prepared composite
films of Fe 2O3 doped ZnO/PS by casting method.
 The focus of this work is to investigate the structural and the optical properties ofthe casted films to get a
material can be easily tun ed for optical application by easier control of the composition.

II. Experimental
Fe2O3 doped ZnOpowder was preparedby combustionmethodthrough mixing zinc nitrate, iron nitrate
and urea as oxidizing agentwith a certain calculated ratios. The mixed powders we re placed in porcelain crucible
to be burned in the furnace at about 370 °C, until the mixture homogenates, self – sustaining and a rather fast
combustion with enormous swelling producing white foamy and voluminous Fe 2O3 doped ZnO. Then, the
temperature of the furnace was increased up to 500°C and the mixture was heated at this temperature for two
hours before the furnace is switched off. Polystyrene (PS)was used as received without further purification
with(MW= 35000 softening point (ASTM 28) 123 -128°C, den sity 1.06 g/mL at 25°C from Sigma -Aldrich,
Germany). The appropriate weight (5gm) of PS was dissolved in 100 ml of chloroform. The mixture was
magnetically stirred continuously at room temperature for 2 hours until the mixture solution has a homogenous
viscous appearance. The solution was left for 3 days before the addition metal oxides filler to it. Different
weights of the prepared powder with (5, 7.5, 10 and 12.5 wt. %) were added to the chloroform and magnetically
stirred vigorously to ensure a high di spersion of the added nanoparticles for 1 hour and then ultra -sonication for
another 1 hour to prevent the nanoparticles agglomeration. The mixture then mixed with the PS solution and
stirred again for1 hour then ultra -sonication for 1 h. The final product of the polymers PS reinforced with Fe 2O3
doped ZnOnanoparticles was cast in glass Petri dishes and left 1 day for drying.
In order to characterize and identify prepared samples, high -resolution transmission electron microscope
(HRTEM) JEM -2100 with an ope rating voltage is 200 keV and gun type is Lab 6 Emmittor was used to analyze
the morphology of the prepared filler. The structure of casted films was characterized by X -ray diffraction
using analytical XʼPert PRO MRD diffract meter system having CuKα (λ =1.540598 Å) with 2θ = 10° – 90°.
The optical measurements of the prepared films were investigated using UV – Vis spectrophotometer type
JASCO 570.
The absorption coefficient of the prepared films was defined by the Beer -Lambert’s law [44] as
𝛼 𝜐 =2.303 ×𝐴𝑏𝑠(𝜆)
𝑑
where d and Abs(𝜆) are the film thickness and the film absorbance, respectively.
The optical energy band gap of the presented films is related to the absorption coefficient by the following
relation [47, 48]:
𝛼 𝜐 ℎ𝜐=𝐵(ℎ𝜐−𝐸𝑔)𝑚
Where Eg, B, and hυ are the optical gap, constant, the incident photon energy, respectively and m is the
index which can have different values of 1/2, 3/2, 2, and 3 depending on the nature of the electronic transition
[49].
The extinction coefficient ( 𝑘) was calculated by the equati on: k= 𝛼λ
4λ
For normal reflectance, the refractive index can be determined from the relation:
𝑛= 1+ 𝑅
1− 𝑅

III. Results and discussion
The morphology of the prepared filler of ZnO doped with Fe 2O3 was investigated by HRTEM. The
photographs of HRTEM reveal a hexagonal crystal structure (wurtzite) of Fe 2O3 doped ZnOnanoparticles as
clearly seen from Fig. (1a). Theparticle size range is from 10 -30 nm. Also the diffraction pattern of the selected
area shown in the inset of Fig.1b reveals a polycrystalline structu re of the prepared powder. The calculated d –
spacing values from diffraction pattern shows all the characterized planes of ZnO; 2.76, 2.69,, 2.45, 1.62 and
1.45 Å are corresponding to the crystallographic planes (100), (101), (002), (110) and (103), respec tively, while
the plane (113) is related to the presence of Fe 2O3.

Tuning the optical properties of Fe2O3 doped ZnO / Polystyrene composite films H. ..
DOI: 10.9790/4861 -100501 4756 www.iosrjournals.org 49 | Page

Fig.(1a -c): HRTEM photographs of Fe2O3 doped ZnO nanoparticles (a) image of prepared nanoparticles& (b)
SAED diffraction pattern

XRD patterns of the casted films of PS filled with different weight percentages of Fe 2O3 doped
ZnO(5, 7.5, 10, and 12.5) are depicted in Fig.(2) . The XRD patterns, reveals that, all the formed peaks is
indexed to the JCPDS card no. 36 -1451, and belongs to the formation hexagonal wurtziteZnO phase with its
characterized planes (100), (002), (101), (102), (110), (103) and (201), but there is no peaks related to the Fe 2O3
as its percentage is less than 5 wt%. Also, the pattern indicates the presence of a hump at 2θ = 10 -20° due to
polystyrene. On the other hand, the XRD shows that the polystyrene has shown some dependence on the
percentage of metal oxides ofFe 2O3 doped ZnO filler ratio certainly, the PS peak is found to increase in
broadness and decreased in intensity. By combining organic and inorganic mate rial, the inorganic nano -sized
particles of Fe 2O3 doped ZnOable to assemble and can stabilize the monomers of polystyrene [40].As the
content of Fe 2O3 doped ZnOin PS matrix increases, the intensity of diffraction peak attributed to PS clearly
decreases. Th is indicates that the Fe 2O3doped ZnOcrystallites are well incorporated in PS matrix. From XRD
pattern, the crystallite size (D) of Fe 2O3 doped ZnOnanoparticles was calculated from the corrected FWHM of
the most intense peak corresponding to (002) plane usi ng Scherrer's formula and it listed in table (1). The
reported data in table (1) explained that the crystallite size decreases with Fe 2O3 doped ZnOcontent from 40 nm
to 18.5 nm.

Tuning the optical properties of Fe2O3 doped ZnO / Polystyrene composite films H. ..
DOI: 10.9790/4861 -100501 4756 www.iosrjournals.org 50 | Page
Fig. (2): X- ray diffraction patterns of Fe2O3 doped ZnO / polystyrene films with different filler concentrations.

Fe2O3 doped ZnO
concentration
5 wt. % Fe 2O3
doped ZnO/PS 7.5 wt. % Fe 2O3
doped ZnO/PS 10 wt. % Fe 2O3 doped
ZnO/PS 12.5 wt. % Fe 2O3
doped ZnO/PS
Crystallite size(nm) 40 31.5 23 18.5
Table (1): The crystallite size of Fe2O3 doped ZnO /PS nanocomposite films

The EDX spectrum of both Fe 2O3 doped ZnO powder and Fe 2O3 doped ZnO/ PS films are shown in
Fig. (3a, b). The characteristic peaks of Zn, O andFe are all found which indicate thepresence of Fe 2O3 as doping
in both powder and composite films, also there is no any impurities in the represented samples.

Tuning the optical properties of Fe2O3 doped ZnO / Polystyrene composite films H. ..
DOI: 10.9790/4861 -100501 4756 www.iosrjournals.org 51 | Page .Fig. (3): EDX images for (a) Fe2O3 doped ZnOpowder & (b) Fe2O3 doped ZnO/ PS films The optical absorption
spectra are very important to understand the optical behavior of the samples. The optical band gap of the
prepared powder ofFe 2O3 doped ZnO can be determined from the relation between the diffuse reflectance (R)
and the wave length (λ) as shown in Fig. (4) . The diffuse ref lectance spectra illustrate absorption response in the
range 400 -600 nm due to the presence of Fe 2O3 as previously reported [41]. The band energy gap value is3.4 eV
which can be deduced from the onset of the linear increase in the diffuse reflectance [42, 43].
400 600 800 1000 1200 14000306090
Fe2O3 doped ZnODiffuse Reflectance(R%)
Wavelength (nm)

Fig. (4) : Diffuse reflectance for Fe2O3 doped ZnO .

The optical absorption spectrum of Fe 2O3 doped ZnO/PS composite films with different concentration
of Fe 2O3 doped ZnOrange from (5 to 12.5 wt %) can be shown in Fig (5) . This figure shows an increase in the
absorption with increasing the concentration of the filler in the PS also with decreasing the wavelength due to
nanocrystalline [44]. The absorbance spectrum shows that Fe 2O3 doped ZnO/PS composite films have two -edge
absorption. The absorptions at lower wavelengths can be attributed to ZnO. The absorptions at the higher
wavelength (visible region) are ascribed to the Fe 2O3 where the band gap energy of bulk Fe 2O3 is 2.2 eV[22 –
26].The absorbance spectrum shows a splitting in the absorption band at 350 nm and 374 nm. The two
absorption bands started to appear with the concentration of 7.5wt%. The splitting in absorption band can be
attributed to the transition of the electrons from the valence to the conduction bands of ZnO [45, 46]. Where the
intensity of these bands increases and become sharper with increasing the addition of Fe 2O3 doped ZnOpowder
in the polymer matrix and a slight shift towards longer wavelengths in the range from 374nm to 376.4 nm. This
observed redshift is an indication of the incorporation ofFe 2O3 into ZnO powder [42, 47].
300 400 500 600 700 8000123456Absorbance
Wavelength (nm) (a) polystyrene
(b) 5 wt% Fe2O3 doped ZnO / PS
(c) 7.5 wt% Fe2O3 doped ZnO/ PS
(d) 10 wt% Fe2O3 doped ZnO/ PS
(e) 12.5 wt% Fe2O3 doped ZnO/ PS
ac de
b

Fig. (5) :UV visible absorption spectra of polystyrene and composites films of Fe2O3 doped ZnO / PS.

Tuning the optical properties of Fe2O3 doped ZnO / Polystyrene composite films H. ..
DOI: 10.9790/4861 -100501 4756 www.iosrjournals.org 52 | Page The optical transmission spectrum of PS and Fe 2O3 doped ZnO/PS nanocomposite films with different
concentration of Fe 2O3 doped ZnOrange from (5 to 12.5 wt. %) can be shown in Fig (6) . This figure explained
that the transmissiondecreased as the Fe 2O3 doped ZnO nanoparticles increased due to the formation of the layer
of covalent bonds formed between Fe 2O3 doped ZnO filler and PS chains lead to decrease in the transmission of
the incident light especially at the shortest wavelengths. The transmittance of pure PS reach to 80% while,
Fe2O3 doped ZnO/PS films shows a decreasing in the transmission.
500 1000 1500 20000102030405060708090
(a) polystyrene
(b) 5 wt% Fe2O3 doped ZnO / PS
(c) 7.5 wt% Fe2O3 doped ZnO/ PS
(d) 10 wt% Fe2O3 doped ZnO/ PS
(e) 12.5 wt% Fe2O3 doped ZnO/ PSTransimision %
wavelength (nm)a
b
cd e

Fig. (6) :UV visible transmission spectra of polystyrene and composites films of Fe2O3 doped ZnO / PS.

Fig (7) shows the relation between the absorption coefficient and the photon energy. The absorption
coefficient α has a small and constant value at low photon energy because of the photon energy is not enough to
transfer the electron from the valence band to the c onduction band (hυ<Eg), while at high energies, the
absorption coefficient increases and hence a great possibility for electron transitions. The absorption coefficient
increases as the concentration of Fe 2O3 doped ZnO nanoparticles at higher energy which i ndicate the crystalline
nature of the samples [48] and as previously discussed from x -ray investigation. So the absorption coefficient
indicates the nature of electron transition, it is expected that indirect transition of electron can occur as the
values of the absorption coefficient are low (α < 104) (cm)-1, as agree with [49]. Also, the absorption coefficient
curves shifts to low photon energy values with increasing Fe 2O3 doped ZnO concentration.
2.0 2.5 3.0 3.5 4.0 4.5 5.00200400600800 (a) Poly Styrene
(b) 5 wt% Fe2O3 dopedZnO /PS
(c) 7.5 wt% Fe2O3 dopedZnO /PS
(d) 10 Fe2O3 dopedZnO /PS
(e) 12.5 wt% Fe2O3 dopedZnO /PSAbsorption Coefficient (cm-1)
h (eV)abcde

Fig. (7) : Absorption coefficient – photon energy relation for all investigated samples.

The allowedindirect energy band gaps of the Fe2O3 doped ZnO/PS composite films are illustrated by plotting
(αhʋ)1/2 versus h ʋ as clearly shown from Fig. (8a -e).

Tuning the optical properties of Fe2O3 doped ZnO / Polystyrene composite films H. ..
DOI: 10.9790/4861 -100501 4756 www.iosrjournals.org 53 | Page

Fig. (8) :Optical band gap values of polystyrene and Fe 2O3doped ZnO /PS composite films as a function of
photon energy.

The energy gap can be obtained by the extrapolated line to the photon energy (h ʋ) axis.The pure PS
shows one indirect optical energy gap while Fe2O3 doped ZnO/PS samples show two indirect optical energy
gaps except for sample with 12.5 wt. %Fe 2O3 doped ZnO. The values of indirect optical energy gap were listed
in table (2).

Concentration Eg1(eV) Eg2 (eV)
PS _ 4.55
5 wt. % Fe 2O3 doped ZnO/PS 2.99 4.25
7.5 wt. % Fe 2O3 doped ZnO / PS 2.94 3.81
10 wt. % Fe 2O3 doped ZnO/PS 2.86 3.76
12.5 wt. % Fe 2O3 doped ZnO/PS 2.82
Table (2): The values of allowed indirect transitionenergy gaps of Fe 2O3 doped ZnO/PSnanocomposite
films.

The obtained energy gap values were found to decrease with increasing concentration of Fe2O3 doped
ZnO in PS matrix. One possible interpretation of this observation is that the insertion of Fe2O3 doped
ZnOnanoparticles in the host matrix introduces multiple states (additional energy levels) in the polystyrene
structure and thus decreasing the band gap energy between the valence and conductions bands. Also, the
decrease of band gap may be due to the strong electronic state exchange interaction. This in teraction leads to
merging the bands belonging to Fe 2O3 and ZnO which in turn reduce the two band into one band as seen for

Tuning the optical properties of Fe2O3 doped ZnO / Polystyrene composite films H. ..
DOI: 10.9790/4861 -100501 4756 www.iosrjournals.org 54 | Page 12.5 wt.%Fe 2O3 doped ZnO / PS sample in table (2). The variation in the value of deduced energy gap was
previously reported [42, 50].
The extinction coefficient as a function of wavelength can be shown from Fig. (9). Thevalue of
extinction coefficient k increases with increasing Fe 2O3 doped ZnOconcentration in the polymer matrix. The
increment of 𝑘 values with wavelength reveals that so me interaction takes place between photons and electrons.
The small extinction coefficient (≈10-4) indicates that the composite samples still are transparent [50, 51], while
the increase in the value of extinction coefficient at higher concentrations indicate higher absorption coefficient.
The variation in the value of extinction coefficient is important in the application of optical devices [52]

Fig. (9): The Extinction coefficient relation with wavelength for the prepared composites films with diff erent
filler concentrations.

Fig. (10a) shows the relation between the refractive index and the wave length. The refractive index for
pure PS film is constant in the range from (200 -800 nm), while it decreases rapidly only at lower wavelengths
range (200 -300nm) for Fe2O3 doped ZnO/PS films and is constant at higher wave length. The values of the
refractive index were taken from the intersection with 𝑌-axis as can be clearly shown from Fig (10b). It is clearly
observed that the refractive index increases as the Fe2O3 doped ZnOwt % increases in PS, this may be
attributed to the increasing the packing density of the investigated films. The small value observed for the
refractive indexes from 1.1 to 1.6is an indication that these composites films are suitable a s low -index claddings
for waveguide applications [53]. The optical properties in this work confirm that the refractiveindex and energy
gap are strongly correlated.

Tuning the optical properties of Fe2O3 doped ZnO / Polystyrene composite films H. ..
DOI: 10.9790/4861 -100501 4756 www.iosrjournals.org 55 | Page
Fig. (10): The refractive index vs. wavelength for the prepared composites films with
different filler concentrations.

IV. Conclusion
 Polymeric films based on polystyrene (PS) filled with different concentration of ZnO doped with Fe 2O3
nanoparticles were prepared by solution casting method.
 Fine scale nanoparticles of wurtzite structure of Fe 2O3 doped ZnOwere investigated by HRTEM and XRD
analysis respectively.
 The optical properties of prepared composite material were performed by means of UV -Vis technique. The
results showed an increase of absorpti on coefficient, extinction coefficient and refractive index with
increasing the percentage ratio of Fe 2O3 doped ZnO nanoparticles in PS matrix.
 Moreover, the calculated optical band gap sharply decreased from 4.54 to 2.82 eV with increasing the filler
percentage.
 Finally, we can conclude that Fe 2O3 doped ZnO nanoparticles addition enhanced the optical properties of
PS. So the composite material will be suitable as low -index claddings for wave guide applications. Also, it
will be suitable for application of photo electronic devices.

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Abomostafa*a " Tuning the optical properties of Fe2O3 doped ZnO / Polystyrene composite
filmsH. .” IOSR Journal of Applied Physics (IOSR -JAP) , vol. 10, no. 5, 201 8, pp. 47-56.

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