Synthesis and optical properties of basic fuchsin dyedoped PMMA polymeric films for laser applications

Opt Quant Electron (2018)50:159
https://doi.org/10.1007/s11082-018-1425-0
Synthesis and optical properties of basic fuchsin dyedoped PMMA polymeric films for laser applications:
wide scale absorption band
M. I. Mohammed1 • I. S. Yahia2,3
Received: 15 November 2017 / Accepted: 7 March 2018
Springer Science+Business Media, LLC, part of Springer Nature 2018
Abstract Basic fuchsin dye-doped poly(methyl methacrylate) polymeric films were sensitized with various dye concentrations ranging from 0.0833 to 1.667 wt% of basic fuchsin.
Their structure, linear absorption, and optical limiting properties were examined. The films
were prepared using a simple and fast casting technique dissolved in chloroform for both
the dye and the polymer. Structural characterizations were achieved by XRD, and the films
showed an amorphous hump supporting the noncrystalline structure of studied polymeric
composites. Spectrophotometer measurements were used to estimate the spectral absorption measurements of the films such as transmittance, absorbance with the calculations of
absorption index (k), and optical energy band gap (Eg) in the wavelength region from 190
to 2500 nm. Results show that the optical constants change with increasing the dye doping
concentrations. It has been found that optical energy gap (Eg) appearing that, both direct
and indirect optical transitions are conceivable for these films. Optical limiting properties
of the films with various dye concentrations were studied using a continuous wave He–Ne
laser operating at 632.8 nm. The results appeared that the sample has an obvious optical
limiting effect. The designed BF/PMMA composites can be applicable in wide-scale
applications.
Keywords Basic fuchsin (BF) dye PMMA XRD Direct and indirect
optical band gap Optical limiting Laser applications
& I. S. Yahia
dr_isyahia@yahoo.com; isyahia@gmail.com; ihussein@kku.edu.sa
1
Metallurgical Lab.1., Department of Physics, Faculty of Education, Ain Shams University,
Roxy, Cairo 11757, Egypt
2
Advanced Functional Materials and Optoelectronic Laboratory (AFMOL), Department of Physics,
Faculty of Science, King Khalid University, P.O. Box 9004, Abha, Saudi Arabia
3
Research Center for Advanced Materials Science (RCAMS), King Khalid University,
P.O. Box 9004, Abha 61413, Saudi Arabia
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M. I. Mohammed, I. S. Yahia
1 Introduction
Organic semiconductor dyes play an extremely role in different criteria and fields in
science, technologies, and engineering for different applications especially absorbing the
visible light for solar cell devices (Zongo et al. 2015; Lee et al. 2015; Kim et al. 2015).
This enforcement takes the help of the inherent power of the dye toward saturating up and
about pastel along with its electrochemical properties after that transfers of electricity by
photosensitive systems (Salmani et al. 2013; Kosa et al. 2012; Zeyada et al. 2015). This
trend is a quickly growing field especially for dye-sensitized solar cells (DSSC) (Zong
et al. 2012; Maia et al. 2012; Makhlouf and Zeyada 2015). DSSC constitutes extremely
applicable as a renewable energy for electric generation from light abortion. It is cheaper
and cost-effective in comparison to the traditional p-n solar cell devices. DSSCs are
considered a most effective cell, cheaper, simple of production, low production technology, for converting the light to electric energy in a large scale (Lin et al. 2015). Most of the
organic materials can conduct as semiconductors suitable for different technology such
solar cells, photo sensors, fluorescence, photoconductive devices (Zhao et al. 2015; Zheng
et al. 2015; Zeyada et al. 2011). The most advantageous point of view of organic over
inorganic semiconductors is the large area of deposition, biodegradable materials, nonvacuum technology, and can be used easily for flexible electronics and optoelectronics.
Basic fuchsin is a triaminotriphenylmethane dye of the triarylmethane family. It is used
on a large scale as a coloring agent for staining of biological tissues, and leather materials
and textiles (Hin and André 2015; Zeyada et al. 2015). Different kind of polymer can be
used as a host for different metal salts and dyes. Polymers can offer some advantages such
as a cost-effective prize, compatibility with dyes for wide scale applications (Ahmed and
Saif 2013; Geetha et al. 2004). Furthermore, polymers become beneficial for sensing
technologies, due to their low-cost materials and their processing techniques being very
simple. In the past decades, it has shown great interest in the material sensor-based
polymer, which appears to change their fluorescence characteristics and absorption to an
external stimulus. For instance of these motive contain deformation, temperature, chemicals, and light, which make the sensors beneficial for a wide variety of technologies
(Crenshaw et al. 2007). Polymer films that including luminescent dyes are utilized as a part
of sensors. To achieve maximum effectiveness of the sensor often chooses polymer-dye
which the dye dissolved in the solvent of the polymer (Lu and Winnik 2001). An
imperative member of the family of poly(acrylic esters) is poly(methyl-methacrylate)
(PMMA). Even though PMMA has a poor heat resistance (Sadek et al. 2011), it has been
utilized as a part of many fields, due to the excellent chemical stability, transparent optical
properties, and great biocompatibility. It may comprise dye molecules to become colorful
and practical. In fact, the integration of dyes to the polymer supports matrices, such as
PMMA and can keep them away from the turbulence in the external environment, which
significantly affect the spectral properties of dyes (Wang et al. 2011).
In this search, we have been studied the effect of basic fuchsin (BF) dye of different
concentrations on the optical properties of PMMA matrix including some measurements
and analysis by diverse techniques and data analysis such as structure analysis by XRD,
absorbance, transmittance, absorption index, optical energy gap and optical limiting. Our
results can be used in a wide scale polymer applications.
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Synthesis and optical properties of basic fuchsin dye-doped…
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2 Experimental techniques
2.1 Preparation of basic fuchsin/PMMA polymeric composite films
Basic fuchsin (BF) named (triamino triphenylmethane) with molecular formula C20H20ClN3, and its molecular structure is given in Fig. 1. The BF doped in PMMA matrix was
prepared by using the casting solution technique. PMMA and dye were dissolved in
chloroform. An appropriate amount of poly(methyl methacrylate) was soluble in a highgrade chloroform on a magnetic stirrer at room temperature for 2 h. Different contents
ranging from 0.0833 to 1.667 wt% of Basic Fuchsia was dissolved in chloroform in situ
with PMMA solution. Casting method was used to prepare BF/PMMA of different BF
contents on the highly cleaned Petri-dish glass. At room temperature, the composite films
(BF/PMMA) were left for 3 days to evaporate off chloroform from them. Acquired films
had been cut into square portions of 2 9 2 cm2 having the thickness 0.5 mm to be
appropriate for further tests and estimations.
2.2 Devices and measurements
The structure of BF/PMMA composite films were investigated by using X-ray diffraction
(XRD) model Shimadzu Lab XRD-6000 with CuKa radiation of wavelength k = 1.5406 Å.
The X-ray system was operated at current = 30 mA and voltage = 30 kV. The diffraction
patterns were preserved using the attached software automatically of a slow scanning
speed equal to 0.02 in the 2h ranging from 5 to 70.
The linear absorption spectra of the films were measured using a double beam spectrophotometer UV–Vis–NIR, JASCO V-570 spectrophotometer in the wavelength extends
190–2500 nm. All estimations were run at room temperature.
To estimate the optical limiting of BF dye-doped PMMA composite polymeric films,
the manual Z-scan technique was used in which the sample is fixed throughout the measuremnets. The most prevalent feature here is to install the sample in the focal length of the
lens inserted between the laser beam and the optical laser power meter. A continuous wave
from a He–Ne laser operating at 632.8 nm was utilized as the excitation source. The focal
lens of 10 cm was settled on the stage of the settled optical bench. Input/output power was
measured by photodetector model (Newport, model-1916R). The holder was designed to
be suitable for the polymeric films.
Fig. 1 Molecular structure
ofbasic fuchsin dye
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M. I. Mohammed, I. S. Yahia
3 Results and discussion
3.1 XRD patterns of basic fuchsin/PMMA polymeric composite films
XRD patterns of BF/PMMA composites with various contents of BF dye were appeared in
Fig. 2. Amorphous structure is recognized for poly(methyl methacrylate (Sava et al. 2002).
Diffraction pattern observed for pure PMMA exhibits a broad diffraction peak at 2h = 14
and another band of lower intensity fastened at 29.7 (Tomara et al. 2011). The form of the
1st-peak meditates the packing of extended polymer chains whereas the 2nd-peak indicates
the ordering within the major chains where their intensity is diminishing methodically
(Hussain and Mohammad 2004). The XRD patterns of the BF/PMMA composites
demonstrate the expansion of the intensity and tightening of the bands of PMMA, whereas,
the remaining part of the diagram stay without any variation. When the dye molecules
integrated into the matrix of the polymer, it may take up the interstitial space among the
polymer chains. For the PMMA composites, the intensity of the peaks at 2h = 14, 29.7
appear of the host matrix PMMA increments, as compared to the unfilled PMMA. This
may be due to the interacting with BF dye molecules. These results are consistent with the
previous studies (Siddiqui et al. 2015; Pan et al. 2009; Kumar et al. 2010).
3.2 Linear optical properties of basic fuchsin/PMMA polymeric composite
films
The optical transmittance spectra as a function of wavelength for several concentrations of
BF dye-doped PMMA is demonstrated in Fig. 3(a, b). The optical properties of pure
PMMA display high transmission through the visible wavelength range over 87% (Maji
et al. 2017) with the absorption peak of PMMA at 266 nm (Maji et al. 2016). The pure
PMMA has high transmittance due to the fact there is no free electron. So, the electrons are
highly attached to their atoms via covalent bonds, i.e., we need photon with high energy to
break the electron linkage and move into the conduction band (Mark 1999). In the case of
Intensity, (a.u.)
1.6667 wt % BF
0.8333 wt % BF
0.1667 wt % BF
0.0833 wt % BF
Pure PMMA
10
20
30
40
50
60
o
2Theta
Fig. 2 X-ray diffraction patterns of BF/PMMA with various dye concentrations
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70
Synthesis and optical properties of basic fuchsin dye-doped…
Page 5 of 12 159
100
(a)
T, (%)
80
60
40
Pure PMMA
0.0833 wt % BF
0.1667 wt % BF
0.8333 wt % BF
1.6667 wt % BF
20
0
300
600
900
1200
1500
1800
2100
2400
, (nm)
100
(b)
80
T,(%)
60
40
Pure PMMA
0.0833 wt % BF
0.1667 wt % BF
0.8333 wt % BF
1.6667 wt % BF
20
0
200
300
400
500
600
700
800
900
, (nm)
Fig. 3 Optical transmittance spectra of BF/PMMA with various dye concentrations as a function of
wavelengths, a in the wavelength range 200–2500 nm, b in the wavelength range 200–900 nm
doped PMMA with BF dye, the polymer transmittance diminishes with increasing the BF
dye contents (Philominal et al. 2012; Mysliwiec et al. 2009). There are three absorption
peaks in the spectrum belong to BF dye at the lower wavelength (k [ 700 nm) region. In
which, the transmission band may be watched in the wavelength & 556 nm whose its
intensity increases with increasing BF dye content (Sreekumar et al. 2011; Wang et al.
2011) and proposing the use of BF/PMMA composites for the optical filter as seen from
Fig. 3b. For the wavelength (k \ 700 nm), the transmission is high, and there are three
absorption peaks take place.
The absorbance spectra for PMMA with different concentration of BF dye are given in
Fig. 4. It is obvious that increment of the concentration of BF dye in the polymer matrix
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M. I. Mohammed, I. S. Yahia
2.0
Pure PMMA
0.0833 wt % BF
0.1667 wt % BF
0.8333 wt % BF
1.6667 wt % BF
Abs
1.5
1.0
0.5
0.0
300
600
900
1200
1500
1800
2100
2400
, (nm)
Fig. 4 Absorbance spectra of BF/PMMA with various dye concentrations as afunction of wavelengths
leads to the increasing of the absorption intensity, and there is no shift in the peak position
for all amounts of BF dye to the polymer. It is clear that the absorption was increased with
the doping level in PMMA polymeric matrix. Such increasing of the absorption supporting
the high interaction of BF with PMMA chains. It means that the BF dye can interact with
the polymer chains and makes more intermolecular bonds (AL-Ahmad et al. 2013). The
increment in the absorption is attributed to the increment of the concentration of BF dye
which represents the absorbing component (Najeeb et al. 2014). It is clear from the spectral
curve that there are various absorption peaks, one in the UV band (& 266 nm) distinguishing p–p* absorption band of PMMA (Zidan et al. 2010) and strong absorption band
with peaks absorption located at 556, 1692, 2250 and 2370 nm. These peaks are characteristic of the chromophoric groups due to the double bond system inside PMMA and BF
groups. The presence of major absorption band in the PMMA composites is related to the
high interaction between BF molecules function groups and PMMA matrix (Kulyk et al.
2016; Nasr et al. 2014).
The absorbance (Abs) for any media can be donating by absorption coefficient (a) of the
incident light. Beer–Lambert’s law can be described as follows for correlation both (abs)
and (a) (Crenshaw et al. 2007; Lu and Winnik 2001):
I ¼ Io eaL ;
ð1Þ
where Io and I are the input and the output light, respectively and L is the thickness of
the polymer sheet. Equation (1) may be recorded as:
a:t ¼ 2:303 log Io =I;
ð2Þ
and we can get
a ¼ 2:303
where
123
Abs
;
t
ð3Þ
Synthesis and optical properties of basic fuchsin dye-doped…
Page 7 of 12 159
Abs ¼ log Io =I;
ð4Þ
It is known that the absorption index (k) is concerned with the absorption coefficient (a)
corresponding to the following relation:
k¼
ak
;
4p
ð5Þ
where k is the light wavelength. Values of the absorption index as a function of wavelengths for various concentrations of BF/PMMA films were studied. Figure 5 explains the
behavior of the absorption index (k) of PMMA with different content of BF dye which
increases with increasing BF contents in the polymeric composites. All the curves have an
absorption peak at 266 nm (characterize PMMA polymer), and another four peaks at 556,
1692, 2250 and 2370 nm for the PMMA/BF absorption curves (Makhlouf and Zeyada
2016). There are a noticeable increase in the values of the absorption peaks with the
increasing of BF-doping. The values of k vary from (0.5 9 10-4 to 1.4 9 10-3).
The optical energy gap is a significant amount to distinguish semiconductors and
insulating material, because of its wonderful status in the design and modeling. The
essential gap: highest occupied molecular orbital (HOMO) to the anti-binding, lowest
unoccupied molecular orbital (LUMO) and the band gap named as (Eg) is the minimal
energy consistency of uncorrelated free electron (separated electron) and hole, related to
the transportation of singular particles in the solid. The Eg values of pure PMMA and BF/
PMMA polymeric composite films are described by Tauc’s law (Tauc 1973):
aht ¼ Aðht Eg Þr ;
ð6Þ
where A is a constant, r = 2 or 3, 1/2 and 3/2 for indirect allowed transition, indirect forbidden transition, direct allowed transition and direct forbidden transition,
respectively. It has been investigated that indirect and direct band gaps of the examined
polymeric films. Figures (6 and 7) show the linear dependence of both (aht)1/2 and (aht)2
on ht and both indirect and direct optical transitions are conceivable for these films. The
straight line portions of the curves are extrapolated to ht = 0 to obtain three optical energy
-3
1.5x10
Pure PMMA
0.0833 wt % BF
0.1667 wt % BF
0.8333 wt % BF
1.6667 wt % BF
Absorption index, (k)
-3
1.2x10
-4
9.0x10
-4
6.0x10
-4
3.0x10
0.0
300
600
900
1200
1500
1800
2100
2400
, (nm)
Fig. 5 Absorption index (k) against the wavelength of BF/PMMA with various dye concentrations
123
159 Page 8 of 12
M. I. Mohammed, I. S. Yahia
Pure PMMA
0.0833 wt %
0.1667 wt %
0.8333 wt %
1.6667 wt %
350
1/2
( h ) , (eV.m )
-1 1/2
300
FB
FB
FB
FB
Eg1(ind)
250
200
150
Eg2(ind)
100
Eg3(ind)
50
0
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
h , (eV)
Fig. 6 The relationship between (aht)1/2 and ht of BF/PMMA with various concentrations
10
1.4x10
Pure PMMA
0.0833 wt % BF
0.1667 wt % BF
0.8333 wt % BF
1.6667 wt % BF
10
1.2x10
2
( h ) , (eV.m )
-1 2
10
1.0x10
9
8.0x10
Eg1(d)
9
6.0x10
9
4.0x10
9
2.0x10
0.0
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
h , (eV)
Fig. 7 Plotting of (aht)2 and ht of BF/PMMA with various dye concentrations
band gaps for jointly direct and direct optical transitions for pure and BF-doped PMMA
films. The band gaps of the studied materials from different regions of the curves in
Figs. (6 and 7), are recorded in Table 1. The optical band gap variations confirm the
presence of additional energy states prompted by dye doping (Abdelrazek et al. 2015).
From this study, the BF dye is modifying the electronic structure as well as the structure of
PMMA due to the formation of defect levels upon doping with efficient BF dye. It
is shown from Figs. (6, 7) and Table 1 that Eg (direct) of PMMA with different content of
BF dye film is located around this values & 5.028–5.092, 3.336–3.357, and
2.051–2.091 eV. It can also appear, that indirect energy gap of pure and BF-doped PMMA
sample is located around these values & 4.774–4.745, 3.1–2.68 and 1.743–1.89 eV and
these values are similar to the value adduced by other workers (Guezguez et al. 2014;
Dorranian et al. 2012; Hussein et al. 2016). With increasing the BF dye contents in PMMA
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Synthesis and optical properties of basic fuchsin dye-doped…
Page 9 of 12 159
Table 1 Optical band gap (indirect and direct) of BF/PMMA with various concentrations
Band gap/polymer
composite
Eg1(ind)
(eV)
Eg2(ind)
(eV)
Eg3(ind)
(eV)
Eg1(d)
(eV)
Eg2(d)
(eV)
Eg3(d)
(eV)
Pure PMMA
4.774
3.100
–
5.028
3.336
–
0.0833 wt% FB
4.765
3.009
1.743
5.106
3.311
2.051
0.1667 wt% FB
4.755
2.968
1.805
5.120
3.301
2.056
0. 8333 wt% FB
4.765
2.999
1.876
5.059
3.305
2.073
1.6667 wt% FB
4.745
2.680
1.890
5.092
3.357
2.091
polymer, the indirect energy gap is decreased due to the presence of dye and their interaction with PMMA and creating new molecular dipoles, which can be considered point
defects produced within the band gap (Esfahani et al. 2014). Nitrogen and Chlorine in the
BF dye has a high electronegativity, which prompts for the low amount of energy band
gap. This outcome values are in a good agreement with that reported before. For example;
it is found that PMMA has optical energy gap for both direct and indirect transitions
(Philominal et al. 2012; Najeeb et al. 2014; Abdelrazek et al. 2015; Sali and Naik 2016).
Also, there are two optical band gaps and two activation energies within the doped PMMA
with 5(6) Carboxyfluorescein dye (Sali and Naik 2016).
3.3 Optical limiting of basic fuchsin/PMMA polymeric composite films
Systems that allow the transmission of ambient light levels with reducing the light
intensity are called Optical limiters. It has been shown that the organic material has a large
nonlinear characterization. The search for optical limiting in organic materials is of
awesome significance. The optical limiting curve for the basic fuchsin-doped PMMA films
with different dye contents is illustrated in Fig. 8. The optical limiting curve illustrates the
0.80
Normalized power
0.75
0.70
0.65
0.60
0.55
0.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
1.6
wt % of BF
Fig. 8 Plot of the normalized power versus the wt% of BF dye using He–Ne laser of 632.8 nm
123
159 Page 10 of 12
M. I. Mohammed, I. S. Yahia
relationship between the normalized power (Normalized power = output power/Main
source power) versus the weight percent of BF doped PMMA polymeric composite films.
From Fig. 8, the value of the normalized power decreases as the dye concentration in the
composite films increases because the samples begin to defocus the laser beam. Higher
concentrations of BF dye in composites, exhibiting clear optical limiting. It is completely
clear for us that the dye concentration plays a substantial part in the limiting optical
property (Manshad and Hassan 2012; Kulyk et al. 2017). The optical limiting characteristics are reinforced with increasing the dye concentrations. This is due to the higher
concentration, and so, the more molecules per unit volume are involved in the interaction.
The results were analogous to the other data reported by other researchers of using low
power optical limiting (Balaji et al. 2011; Iliopoulos et al. 2012; Badran and Hassan 2011).
According to these experimental results, this dye is a promising material for many
applications in nonlinear media (Vinitha et al. 2009; Aithal et al. 2016). It is also considered the limiting amplitude is increased with increasing the dye concentrations in the
studied samples in this work (Pathrose et al. 2016).
4 Conclusion
From this study, it can be inferred the modulations in structural, linear absorption and
nonlinear absorption of basic fuchsin doped PMMA. XRD technique assures that the
composite films own the amorphous nature. The spectrum of composite films containing
various absorption peaks, one of them characterized by PMMA polymer while the others
belong to the basic fuchsin dye-doped PMMA. With increasing the dye concentration, the
intensity of the peaks increases. The analysis of optical energy gap showed the existence of
three optical band gaps for BF/PMMA. These variations in the band gap with doping were
understood by invoking the existence of defect levels within the BF doped PMMA films.
As the concentration of the dye increase, the absorption index is also increased. The optical
limiting activity showed a concentration-dependent. BF/PMMA polymeric films can be
used in nonlinear media, optical limiters, and photonic devices.
Acknowledgements The authors are grateful to the Research Center for Advanced Material Science
(RCAMS) at King Khalid University, with Grant Number (RCAMS-1-17-5).
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