Resonant Measurement Piezoelectric Materials

114 Figure 5-4: Comparison of sample D and C series for the value of capacitance over the ratio of areathickness with ± 5 error. The resonant and antiresonant frequencies that correspond to the minimum and maximum impedances of the materials are important variables to determine the piezoelectric constants of the materials. The frequency response of the samples was measured by using NetworkSpectrum Analyser HP 4195A between 100 kHz to 500 MHz. The resonant and antiresonant frequencies for sample D series can be identified by the magnitude of the impedance as shown in Figure 5-5. There are a few possible modes of vibration in the range of 120 kHz to 280 kHz: lateral, longitudinal and thickness modes. For all the samples of series C and D, the thickness vibration mode is not significant compared to the lateral and longitudinal modes. This is due to the fact that the length and the width of the samples are more than 50 times bigger than their thickness. The lateral vibration mode was observed for samples D1 and D2 which is about 180 kHz, however, the lateral mode diminishes as the length of the sample increases which can be see in sample D3 – D5 as shown in Figure 5-5. The resonant frequency of the longitudinal mode for sample D1 is about 240 kHz and reduced to about 185 kHz for sample D5. From equation 2-4, the average value of d 31 for sample D series is about 33.9 pCN. 115 Figure 5-5: Frequency response for sample D1, D2, D3, D4 and D5, corresponds to their impedance. Sample D1 Sample D2 Sample D3 Sample D4 Sample D5 116 Similar to the case of sample D series, Figure 5-6 shows the frequency response for sample C series. Sample C2, which has a square dimension displays two significant vibration modes. One of which is the lateral mode, at a resonant frequency of 165 kHz and the other one is the longitudinal mode, which happens at around 235 kHz. For sample C1, with its length smaller than its width, the lateral mode occurs at the resonant frequency similar to sample C2, at 165 kHz, due to the fact that their dimensions are almost similar which results in poor output from longitudinal vibration mode. As the length of the sample increases and becomes larger than its width sample C3, the longitudinal vibration mode becomes prominent which happens at a resonant frequency of 178 kHz, while the lateral mode diminishes as the length of the sample increases. The resonant frequency is inversely proportional to the length of the material, as shown in Figure 5-7, which is in good agreement with equation 2-4. The average value of d 31 for sample C series is 24 pCN, which is slightly smaller than sample D series. Figure 5-6: Frequency response for sample C series. The longitudinal resonant frequencies of sample D and C series are inversely proportional to the length of the structure as indicated in Figure 5-7, which is consistent with equation 2-7. The elastic compliances at constant electric field, s 11 E for sample D ranges from 5.48 × 10 -12 m 2 N to 12.9 × 10 -12 m 2 N and ranges from 5.85 × 10 -12 m 2 N to 13.4 × 10 -12 m 2 N for sample C series, with the assumption that, the density of PZT type-5H is 7400 kgm 3 [31]. 100 200 300 400 500 120 140 160 180 200 220 240 260 280 Z m O h m Excited Frequency kHz C1 C2 C3 117 Figure 5-7: Resonant frequency as a function of inverse of cantilever length. The coupling factor for the material can be estimated by substituting the measured values of d 31 , and into equation 2-6. Figure 5-8 shows that the coupling factor increases with length of the materials. For example, the coupling factor for sample D series increases from 0.127 at a length of 6.75 mm to 0.216 at a length of 18 mm, while sample C series has a slight reduced coupling factor of 0.12 at a length of 6.75 mm and increases to 0.192 at a length of 13.5 mm. Figure 5-8: Coupling factor of sample D and C series as a factor of material length. From equation 2-8, the constant displacement elastic compliance, s 11 D for sample D series ranges from 5.1 × 10 -12 m 2 N to 12.6 × 10 -12 m 2 N, while that for sample C series 118 ranges from 5.63 × 10 -12 m 2 N to 13.3 × 10 -21 m 2 N. The piezoelectric charge coefficients calculated from equation 2-9 for samples D and C series range from 9.38 × 10 -3 VmN to 11.4 × 10 -3 VmN and 8.3 × 10 -3 VmN to 9.1 × 10 -3 VmN, respectively. As expected, the impedance reduces as the length of the material increases as shown in Figure 5-9. The minimum impedance impedance at resonant frequency is proportional to the ratio of thickness to the area of the material. The impedances at resonant frequency were measured for evaluating the mechanical quality factor, Q m of the materials according to equation 2-10. The mechanical quality factor for the samples was calculated and plotted in Figure 5-10. On average both samples have a Q-factor, Q m of the order of 120. The experimental results obtained by the resonant measurement method for all the piezoelectric properties are summarised in Table 5-2. Figure 5-9: The impedance at resonance is proportional to the ratio of thickness to the area of the material. 119 Figure 5-10: Mechanical quality factor, Q m for sample C and D series. Table 5-2: Summary of measurement results from resonant measurement method for sample C and D series. Piezoelectric Constant C D C1 C2 C3 D2 D3 D4 D5 Constant electric field elastic compliance s 11 E  10 -12 m 2 N 13.4 10.2 5.9 12.9 9.9 7.6 5.5 Constant displacement elastic compliance s 11 D  10 -12 m 2 N 13.3 10.0 5.6 12.6 9.5 7.2 5.1 Permittivity  10 -9 Fm 2.9 2.6 2.6 3.6 3.3 3.1 3.0 Relative dielectric constant K 33 T dimensionless 325 295 295 4.8 372 347 336 Coupling factor k 31 dimensionless 0.12 0.15 0.19 0.16 0.19 0.22 0.27 Piezoelectric charge coefficient d 31  10 -12 CN -29 -26 -21 -39 -32 -25 -22 Piezoelectric voltage coefficient g 31  10 -3 VmN -8.3 -9.1 -9.1 -9.4 -10.3 -11.0 -11.4 Impedance at resonance Z m Ω 205 188 90 162 103 88 75 Mechanical quality factor Q m dimensionless 99 89 125 100 103 138 130 120

5.5 Direct Measurement Berlincourt Method

The piezoelectric charge coefficient, d 33 can be measured directly with a commercial Berlincourt piezometer system www.piezotest.com, as shown in Figure 5-11 a. The piezoelectric specimens were obtained by detaching the free-standing part of the samples from their base on the substrate. The specimens were then inserted in between a loading contact of the piezometer system as shown in Figure 5-11 b. A continuous alternating force is applied on the specimen resulting in production of charges, corresponding to the d 33 piezoelectric effect. The magnitude of the measurement result is a ratio of short circuit charge density over the applied stress, according to equation 2-2. Figure 5-11: A photograph a and a schematic diagram b showing a piezoelectric specimen being measured with the Berlincourt measurement method.

5.5.1 Effect of Substrate Clamping

Conventionally, thick-film piezoelectric materials are printed on a rigid support substrate. This rigidly clamps the films to the substrate and imposes a deformation restriction on the lower surface of the films when stress is applied as shown in Figure 5-12. There are a few possible types of mechanical clamping for a film printed on a substrate [84]; one of which is where the piezoelectric film is mechanically bonded with an inactive substrate. With the presence of the substrate, an interfacial stress occurs between the printed piezoelectric film and the substrate and causes the measured effective piezoelectric coefficient d 33 to reduce from the true value [82]. This is because a b Static Pre-load Loading Contacts Load Cell AC Loading Unit Piezoelectric Specimen 121 of the influence of the d 31 component in the film when a deformation of the structure occurs. Figure 5-12: Diagram of a free-standing film in expansion a and contraction b compared to a clamped film in expansion c and contraction d. Theoretical analysis [82] shows that a reduction of measured d 33 is inevitable for a clamped sample according to 5-1 By substituting the parameters for the properties of an alumina substrate and a clamped thick-film as listed in Table 5-3 into equation 5-1, the unclamped d 33 can be estimated, which is slightly more than 80 compared to the measured value of a clamped sample. Another problem associated with the determination of d 33 is the fact that the system of substrate-piezoelectric film acts as a natural bending element. Therefore, to determine d 33 correctly, the change in thickness of a specimen between two opposite points at the upper and the lower side of the sample must be measured [84]. Free-standing films are not completely free from the clamping effect: for example, the electrode itself may cause a mechanical clamping. However the thickness of the electrodes is much smaller than the piezoelectric films and furthermore the elasticity of AgPd electrode is greater than the piezoelectric film, therefore the clamping effect of the electrode-PZT can be neglected [84].     2 12 11 13 31 33 33                       E E E su b str a te su b str a te u n cla mp ed cla mp ed s s s e d d d  a c b d