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Facile Formation of β Poly (vinylidene fluoride) Films using the Short Time
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Advances in Environmental Biology

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Facile Formation of β Poly (vinylidene fluoride) Films using the Short Time
Annealing Process
1,2Ibtisam
Yahya Abdullah, 1Mohammad Hafizuddin Haji Jumali, 1Muhammad Yahaya, 1,3Haider

Mohammed Shanshool
1
School of Applied Physics, Faculty of Science and Technology, UniversitiKebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia
2
Department of Physics, College of Science, University of Mosul, Iraq
3
Ministry of Science and Technology, Baghdad- Iraq

ARTICLE INFO ABSTRACT

Article history: Background: This work reports the effect of annealing temperatures on the crystalline
Received 25 July 2015 structure of poly(vinylidene fluoride) (PVDF) film. The solution of PVDF/DMF
Accepted 30 August 2015 deposited onto a glass substrate by spin-coatedto form a film of 10µm in thickness. The
Available online 9 September 2015 film is annealed at different temperatures at 30 minutes. The crystalline structure of the
films investigates using XRD and FTIR techniques while the morphology determine
Keywords: using SEM. It observes that the dissolution of PVDF in DMF followed by spin-coating
Annealing,β-phase, morphology, spin onto a glass substrate changed, directly, from alpha to beta phase which confirm by
coating, piezoelectric, PVDF XRD and FTIR. The analyses of SEM show the surface is rough, porous and spherulites
structure. They're moderately increasing of β-phase content that is equal 47% as PVDF
powder to 76% as PVDF thin film. However, subsequent annealing process enhance the
formation of β-phase suggesting the importance of this step.

© 2015 AENSI Publisher All rights reserved.

To Cite This Article: Ibtisam Yahya Abdullah, Mohammad Hafizuddin Haji Jumali, Muhammad Yahaya, Haider Mohammed Shanshool,
Facile Formation of β Poly (vinylidene fluoride) Films using the Short Time Annealing Process. Adv. Environ. Biol., 9(20), 20-27, 2015

INTRODUCTION

Poly(vinylidene fluoride) (PVDF), as piezoelectric polymer, has been extensively investigated since a many
years ago. This is because, PVDF exhibits outstanding electroactive properties compare to otherpolymers. As a
polymer, it is not surprising thatPVDF has been recognized as the green solution to a more toxic Pb based
ceramics for sensor and actuator applications. Besides excellent pyro and piezoelectric properties, PVDF
exhibitsa combination of other good properties such as easyprocessability,good mechanical and chemical
stabilityas well as low mechanical and acoustic impedance.PVDF exists in five different phases, namely α, β,
γ,δand ε phases. The excellent electroactive properties of PVDF, however, depends strongly on the amount of β-
phase in the material[1,2].This is because, theβ-phase having planer zig-zag arrangement exhibits the highest
dipole moment per unit cell as compared to γ and δ phases, while α and ε phases are non-polar[3,4]. Thus,it is
admirable to produce PVDF with β (and γ) phases due to itsenormous benefits in sensors and actuators.
In general, the existence of phases in PVDF is strongly influenced by processing and fabrication
parameters. There are severalmain parameterssuch as type of solvent[5, 6]melting temperatures[6,7]casting
techniques[8],mechanical deformation[9, 10]and annealing temperatures[11, 12] although other influencing
parameters were also investigatedsuch as melt under specific conditions such as high pressure[13, 14], external
electric field[15, 16]and ultra-fast cooling[12, 17].Although there are numerous works describing the methods to
produce the β-phase, but they were done in many consistent steps. Moreover, there are many interrelated
parameters and thus it is common to find reports suggesting multiple steps combining two or more factors.
Consequently, the procedure becoming more complicated and susceptible to even a small variation. For
example, although solventsuch as dissolution is followed with other steps such as cast methods[8] and
annealing[11, 12].
Previous works claimed that high content of the β-phase in PVDF films prepared using the casting method
was successfully produced after a long annealing process[11, 12]. The casting method produces an irregular film
with high thickness which needs a long time to dry. The annealing process at high temperatures increases the
ability of the polymer chain to move and thus improved crystallization. The increase in crystallization via an
Corresponding Author: Ibtisam Yahya Abdullah, School of Applied Physics, Faculty of Science and Technology,
Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia.
Tel: +61123081862. E-mail: ibtisamyahya@yahoo.com
21 Ibtisam Yahya Abdullah et al, 2015
Advances in Environmental Biology, 9(20) Special 2015, Pages: 20-27

annealing process depends on the annealing time and annealing temperature. In this work, the crystalline
structure of the PVDF investigate as a function of annealing temperature and using DMF as a solvent on order to
enhancement the β-phase in the PVDF.The PVDF films were prepared by the spin coating technique and
annealed at different temperature namely, 50, 70, 90 and 110oCfor 30 minute by using oven and addition to the
room temperature 30oC. In spite of use simple method and short annealing time, a high content of the β-phase is
achieve compare by previous works which suggesting that a minimum of five hours is necessary for annealing
process to obtain the β- phase at 90oC[12, 11] by using cast method. The morphology of the PVDF films studied
by scanning electron microscopy SEM. The phase of the PVDF powder and films were measured with X-ray
diffraction (XRD) and Fourier transforms infrared (FTIR) spectroscopy.

MATERIALS AND METHOD

Initially the PVDF(in powder form) received from SIGMA-ALDRICHwas dissolved in N,N-
dimethylformamide (DMF 99.5%) to form a PVDF solution with a concentration of 15wt %. The solution was
continuously stirred using a magnetic stirrerfor 30 minutes at 60oC.Approximately0.1ml of the PVDF solution
wasdropped on toa clean glass substrates (2.5x2.5cm2)and thenspin-coatedto form a film. In this work, the spin-
coating parameters namely,angular velocity and duration were fixed at 1000 rpm and 30seconds, respectively.
Subsequently, the PVDF films were annealed atdifferent temperatures namely room temperatures:30oC,50, 70,
90 and 110oCfor 30minutes.

Characterization:
The morphology and thicknesses of the films wasdetermined using scanning electron microscopy (SEM)
model ZEISS EVO MA10. The samples were gold plated before SEM observation. Thephases of thesamples
were determined byusing a Bruker D8 Advancediffractometerwhich operated at 40kV and 40mA and produced
aCuKα1 wavelength of 0.15406nm. The peaks were recorded in the 2θ range of 10°–60°.In addition, the Fourier
transformation infrared spectroscopy (FTIR)was used to confirm the phase of all samples. The FTIR spectra of
the sampleswere obtained in a Perkin Elmer spectrum, with a resolution of 4.00 cm-1 over a range of 650-
4000cm-1.

RESULTS AND DISCUSSION

Sem analysis:
Figure 1 shows the SEM micrographs with different magnification of the PVDF films at room temperature
30oC and at annealing temperatures 50, 70, 90 and 110 oC. The analysis of SEM micrographs was done by using
ImageJ analyzingsoftware 1.49r. It is clear that the surface of all samples appeared rough, porous and contained
spherulites but the size of spherulites, and distribution were not homogeneous.Diagram1shows the variation in
the porous and the size of spherulites in the PVDF films. The porosity has different percent with variation of
temperature. At room temperature 30oC, the porosity was 91.92%. By increasing the annealing temperature, the
porositydecrease until reached the values 82.66% at 110oC (Diagram 1.a). The porosity depends on the
evaporation rate of the solvent[11] which in turn inverse proportional to the boiling point of solvent (153oC for
DMM), where, the higher boiling point the lower evaporation rate[18]. That means the lower evaporation rate of
the solvent caused lower sample porosity. The formation of β-phase favored at low evaporating while high tares
preferred to formation the α-phase. In PVDF film applications, the porosity reduced the mechanical strength of
these films performance them little ductile.Also, the high porosity may be effect to the polarization process
which encumbering the polarization process through break at relatively low electric fields.These results obtained
in this work conflict with the results of Cardoso and coworkers[19] which obtained smooth and flat surface
between 30 and 80◦C.The size ofspherulites differ with different temperature (Diagram 1.b). The spherulite size
reflect the crystallization kinetics of the polymer[20]. At 30oC, the spherulite size was (700.10nm in diameter)
which has the largest value and decreased with increasing the annealing temperature to become 610.83nm at
110oC. This perhaps occurs due to the variation on the rate of nucleation and growth, where by increasing the
annealing temperature the nucleation rate decrease and an increase in the growth rate of these spherulites[21].
Gregorio and Borges[8] mentioned thatthe spherical structures with small diameter refer to the formation of the
β-phase whereas the radial lamellae refer to the formation of the α-phase.Gregorio and Borges[8] shows that the
size of spherulites increased with increasing temperature and the porosity was reduced.
Figure 1 shows the cross-section of the PVDF films prepared in this work. The range thicknesses of the
films wereapproximately 7µm-10µm. Cross section measurements also emphasized the naturalness of all
samples in term of roughness and porosity. It was noted that surfaces were irregular, and contained a non-
homogeneous distribution of spherulites and the top and bottom of the samples were not uniform. All films
exhibited highly inhomogeneous structures owing to the presence of voids of different size and shape
22 Ibtisam Yahya Abdullah et al, 2015
Advances in Environmental Biology, 9(20) Special 2015, Pages: 20-27

surrounded by agglomeration of spherulites between the upper and lower layers. The size of spherulites appears
different in each sample.

Xrd analysis:
Figure 2 shows the XRD diffractogram of the PVDF powder sample and thin films. In PVDF powder figure
2.a, there were three prominent peaks observed at 2θ=18.4o (020), 19.8o(110) and 26.4o(021)confirming that the
originalphase of PVDF used in this workwasα-phase[22]. Figure 2.b shows the X-raydiffractogram of PVDF
filmsprepared in this study. Generally, the samples diffractograms consisted of a dominant peak at 2θ=20.2o
(200/110), 20.3o(200/110) and 20.4o(200/110) which all attributed to the β-phase,and two broad peaks. The first
broad peak was located approximatelybetween17.9o and 26o2θwhile the second peak appeared at a 2θ range of
30o-45o. It is important to note that in all X-ray diffractions for the films, the complete disappearance of a
reflection peak located at 26.0o as observed in a powder sample. This observation signifiedthat a major
structural change hadtaken place. Moreover, a distinguished peak located at 18.4o as a signature of α-phasewas
transformed into a broad peak offering additional evidence of structuralmodification.
Detailed analysis of the diffractogramsrevealed the prominent peak was located at 2θ=20.8o (110)[23].In all
the diffractograms, this peak appeared as the main peak, suggesting the creation of a β-phase in the material.
Since this peak was quite broad, it strongly overlapped with the remaining α-phase.
One of the important parameters to enhance the crystallization β-phase in PVDF is the molecular interaction
between the PVDF and solvent. In the case of DMF as a solvent, the molecular interaction include the dipolar
interactions between C=Oand CH2–CF2 in DMF and PVDF respectively, and the presence of weak hydrogen
bonding C=O….H–C, both of which disrupt the inter-chain forces of solid PVDF and finally dissolve the
PVDF[24,25].
The polarity of the solvent has an effect on the crystalline of the PVDF. High polar solvents cause the
strong dipoles of the molecular chain C–F bond in the PVDF to rotate and decrease the energy barrier for
creating the more expanded all trans conformation (TTT) ,whereas solvents with a lower dipole moment always
favors alternate trans and gauche conformation (TGTG)[26, 27]. However, using the same polar solvent can
fabricate various phases depending on the temperature of the preparation[28] and evaporation of the
solvent[29].The presence of α, β and γ phases in the PVDF for a specific polar solvent depends also on the
mobility of conformers which are mostly affected by thermal energy[21].
When the PVDF crystallizes from the solvent, the molecular chains have no fixed structure and can move
around freely. The dissolution of aPVDF crystalline regions required interaction energy of the polymer-solvent
to go beyond that between the polymer chains. At low temperatures, the reaction energy between polymer
molecular chains are greater than the reaction energy of interact polymer-solvent, so the crystalline region of the
PVDF remain practically interactive and swelling results, as the solvent succeeds to enter the amorphous region.
At high temperatures, the reaction energy of polymer chain reduction and the solvent succeedto penetrate the
crystalline region, causing complete or partial dissolution.
When the solution deposits on the substrate, the solution solidifies, the crystalline phase of the PVDF
depends on the rate of crystallizationand according, on the rate of solvent evaporation. Chinagliaand
coworkers[29]found that low evaporation rates favoredthe formation of the β-phase, whereas high rates resulted
mainly in α-phase. The process of crystallization of PVDF starts with nucleation which in turn consists of two
steps, the formation of liquid-like clusters of PVDF molecules and the rate-limiting organization of such clusters
into crystal nuclei[30].So, in this work the phase formed by using DMF as a solvent for PVDF was the β-phase.

Ftir analysis:
According to previous works[31], the peaks of theα,β and γ-phase are demonstrated in Table 1.The 840 cm-
1
band is common to the β and γ-phases; a sharp and well-resolved band indicates the β-phase, whereas a broad
band indicates the γ-phase. This broad band is due to superimposition with the 833 cm-1 band which often
appears as a shoulder[32, 33].The second evidence which characterizes each of β (TTT) and γ-phase (TTTG) in
PVDF existence the peaks at 1276 identified the β-phase and 1232cm-1belong to γ-phase, the β and γ-phase look
alike each other structurally and spectroscopically due to the existence of TTT in the chain conformation in both
γ and β-phases giving rise to some common vibrational bands such as at 841 and 510 cm-1.
FTIR spectra of the PVDF powder and thin films shown in figure 3 in the range of 600–1600 cm–1. The
absorption band of the PVDF powder (figure 3.a) confirmed the existence of α-phase as a dominant phase (762,
796and 975). The band vibration of 762 belonged to CF 2 bending and skeletal bending mode. The bands at 796
and 975 ascribe to the CH2twisting mode. FTIR spectra of PVDF films (figure 3.b) at room temperature 30°C
and annealing condition at 50, 70, 90 and 110°C for 30 minutes, respectively. There was no difference to
distinguish to all of the PVDF films. The peaks at 840, 876, 1071, 1171, 1272, 1401 and 1429 that appeared in
this figure represent the β-phase. The peak at 840 in β-phase was sharp with high intensity while in γ-phase, the
peak was broad and low intensity. So in this work the peak at 840 was sharp and high intensity as shown in
figure 4.b. From comparison the FTIR results of the thin films with powder, its show disappearance the peaks
23 Ibtisam Yahya Abdullah et al, 2015
Advances in Environmental Biology, 9(20) Special 2015, Pages: 20-27

that appear in the α-phase namely, 762, 796 and 974 in the PVDF films. So, this indicates to transfer the phase
of the PVDF from α to the β-phase. Consequently, the FTIRconformed the XRD results to transfer the phase of
PVDF.The IR vibration of the PVDF films is 840cm-1 thatwas assigned to the CH2 rocking mode, 874 and
1071 was assigned to the CC skeletal stretchingvibration, 1171(CF2 out-of-plane deformation), 1401cm-1 was
assigned to the CF2 wagging mode and 1429cm-1 to the CH2 bending.
FTIR technique was also used to determine the contents of a β-phase in each sample. The following formula
wasused to calculate it[34, 35].

Table 1: FTIR Transmission Spectra (cm-1) for the phases of PVDF Film Sample[31]
α β γ
764 840 840
795 881 880
872 1074 1073
974 1172 1176
1152 1406 1234
1183 1405
1214
1382
1405

Fig. 1: SEM& Cross SectionMicrographs with Different Magnification of the PVDF Films: a-30oC, b- 50oC, c-
70oC, d-90oC and e-110oC
24 Ibtisam Yahya Abdullah et al, 2015
Advances in Environmental Biology, 9(20) Special 2015, Pages: 20-27

𝐴𝛽
𝐹𝛽 =
1.26𝐴𝛼 + 𝐴𝛽
whereAα and Aβ are the absorption fraction at 763 and 840 of α and β-phase, respectively.Diagram 2 shows
the β-phase content of the PVDF powder and thin films. It appears that the β content in the PVDF powder is
47%. In the case of thin films, the ratio increases with increasing annealing temperatures and has high values
of76% at 110oC.

Conclusions:
This study demonstratedthe effect of the annealingprocess on the crystalline phases of PVDF. This subject
is relevant as the material has interesting properties for applications, such as sensors, which may be subjected to
different temperatures. PVDF films were fabricated by using the spin-coating method. The annealing at 50, 70,
90 and 110oC for30 minutes and at room temperature 30oC,make a decision the presence of the β-phase in
PVDF films by using the same polar solvent.The morphology of sampleswas investigated using SEM.It
appeared that the surface of samples wasrough and porousand contained spherulites. Therefore, the annealing
processhadan effect on the microstructure of samples. The XRDdiffractogramshowed that the primary phasein
PVDF powder wasα-phase and transformed to theβ-phase when crystalline films formed PVDF/DMF. The
phase formed was influenced by the crystalline rate and the evaporation rate of the solvent in addition to the
effect of temperature.The FTIR spectra confirmedthe XRD that the PVDF films were converted from α-phase to
the β-phase and the β-phase content increase from 47 in the PVDF powder to become76% in the PVDF thin
films.

Diagram 1: The Variation of the (a) Porosity and (b) Size of the Spherulites in the PVDF Films at Different
Temperatures

Fig. 2: XRD of the PVDF (a) Powder and(b)Thin Filmsat Different Temperature.
25 Ibtisam Yahya Abdullah et al, 2015
Advances in Environmental Biology, 9(20) Special 2015, Pages: 20-27

Fig. 3: FTIR for the PVDF (a) Powder and(b)Thin Films in the Wavenumber Region of 400 to 1600 cm-1at
Different Temperature

Diagram 3: β-phaseContent for the PVDF Powder and Thin Films at Different Temperature.

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