3.1 Surface morphology
The P(VDF-TrFE)/ZrO2 and P(VDF-TrFE)/TiO2 nano composites thin-film surface morphology and nano particles allocation of are examined by Scanning Electron Microscopy (GEMINI Ultra FE-SEM, carl Zeiss). The well dispersed nano particles ZrO2 and TiO2 presents in composites at 1µm region are shown in Figure1 (a-b). Energy Dispersive Spectrometer spectrum - EDS (GEMINI Ultra FE-SEM, carl Zeiss) confirm the presents ZrO2, TiO2 in polymer matrix and shown in Figure 1c to 1d. ZrO2 /P(VDF-TrFE) film, Zr obtained at the energy level of 2Kev and TiO2 /P(VDF-TrFE) film, Ti obtained at the energy level 4.5 Kev. Fluorine, Oxygen and carbon energy signal emissions at the energy level of 0.5 KeV, 0.6 KeV and 0.24 Kev respectively [15-16].
3.2. FTIR
The ceramic nanomaterial ZrO2 and TiO2 with P(VDF-TrFE) nano-composites piezoelectric properties and molecular bonding are confirmed by Fourier Transform - Infrared Spectroscopy (Thermo fisher Scientific FTIR spectrophotometer (Nicolet 6700 FT)) measurement and shown in Figure 2. The FT-IR measurement of ZrO2/P(VDF-TrFE) and TiO2 /P(VDF-TrFE) nano-composite film obtained transmittance peak at 841 cm-1 (CH2 rocking) , 1288 cm-1 (Trans band) , 1400 cm-1 (CH2 Wagging) are confirms the β-phase. [17-19]
3.3. XPS (X-Ray photoelectron Spectroscopy)
The ZrO2/P(VDF-TrFE) and TiO2 /P(VDF-TrFE) nano-composite film, chemical composition and binding energy are confirmed by X-Ray photoelectron spectro scopy (Axis Ultra DLD, Kratos Analytical UK with AlKa as the radiation source (hv = 1 .486 KeV), 15 kV, and 10 mA). A wide spectrum analysis of each ceramic nano-composite materials elements are shown in Figures 3.a and 3.b. In these wide spectrum analysis Oxygen (O1s), Carbon (C1s), Fluorine (F1s) elements are obtained and it’s strong peaks in the energy level of 531e.V, 285 e.V, 686 e.V in the energy range of 100 eV to 800eV. The ceramic fillers ZrO2 and TiO2 molecular elements Zr 3d5/2, Zr 3d3/2 , Ti 2p3/2, Ti 2p1/2 energy levels 182.9 e.V, 185 e.V, 459.2e.V, 464.1e.V are clearly shown Figures 3.c and 3.d. [20-22]
3.4 AFM (Atomic Force Microscopy)
The Atomic Force Microscopy (Bruker, Germany) surface image of nano composite thin-film and surface roughness of ZrO2/ P(VDF-TrFE) and TiO2/P(VDF-TrFE) are presented in Figure. 4 (a-b) and Figure.5 (a-b). The Ra, Rq, Rp and Rz values are measured at average range of 50µm line area from AFM image using Gwyddion software [23-24]. The height of the TiO2 nano particles value is high compare with ZrO2 nano particles. The Ra, Rq, Rp and Rz values of ZrO2/P(VDF-TrFE) composite thin film are double time lower than the TiO2/P(VDF-TrFE) composite film are presented in the Table 1.
Table 1. Surface roughness Parameters
S.no
|
Parameters at 50µm
|
TiO2
(nm)
|
ZrO2
(nm)
|
1
|
Ra
|
23
|
10
|
2
|
Rq
|
28
|
13.5
|
3
|
Rp
|
76
|
47
|
4
|
Rz
|
139
|
58
|
3.5 LDV (Laser Doppler Vibrometer)
The velocity of cantilever beam measured by using noncontact Laser Doppler Vibrometer (LDV) with respect to the time. By using Fast Fourier Transform (FFT) the resonance frequency is calculated through measured velocity. The Velocity Vs Time signal and Frequency Vs Magnitude graphs are shown in Figures 6(a-b) and 7(a-b). The obtained resonance frequency of ZrO2/P(VDF-TrFE) and TiO2 /P(VDF-TrFE) are 64 Hz and 52.7 Hz respectively [25].