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Evaluation of Piezoelectric Parameters of Several Commercial Thick Film Capacitor Dielectrics

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Evaluation of Piezoelectric Parameters of Several Commercial Thick Film Capacitor Dielectrics European Microelectronics 10-13 September 2017, Warsaw, Poland Packaging Conference www.empc2017.pl Evaluation of Piezoelectric Parameters of Several Commercial Thick Film Capacitor Dielectrics Artem Ivanov Faculty of Electrical and Industrial Engineering Landshut University of Applied Sciences Landshut, Germany [email protected] Abstract—Piezoelectric properties of several high-K dielectric response must also be known. In the constructed experiments the pastes from ESL ElectroScience were investigated. The absolute generated charge in typical sensor configurations (normal load values of measured piezoelectric coefficients d31 range from below and bimorph bending) was measured. This charge signal can be of 1 pC/N to more than 50 pC/N. The aging rates of piezoelectric used directly to find achievable sensor properties like signal response are shown to be substantially higher than of typical amplitude and signal to noise ratio. Additionally, piezoelectric piezoelectric materials. Measurements of high-field hysteresis coefficients were calculated from the generated charge using loops together with low-field dielectric parameters and their methods described below to allow a better comparison with temperature dependence were performed. Achieved piezoelectric typical piezoelectric materials. response of samples as function of temperature, electric field strength and duration of polarisation was measured. Results A preliminary elemental analysis performed on the base of concerning the Curie temperature and the initial polarization of X-Ray fluorescence spectra showed that the dielectrics are built the samples are also presented. with Bi/Ba/Zn, Pb/Ga and Pb/Nb/Ga systems. It is known from the literature that the Curie temperature of Pb/Nb systems can be Keywords—piezoelectric effect; capacitor dielectric; thick film as low as –15°C [2], which would prohibit any practical paste; screen printing piezoelectric applications. That is why the measurement of the Curie temperature of the dielectrics was one of the goals during I. INTRODUCTION the investigations. Thick film capacitor dielectric pastes with relative permittivity in the range of up to 12000 are commercially II. SAMPLE PREPARATION available for about two decades [1]. Most of these pastes are Samples were screen printed on 96% alumina substrates with compatible with standard thick film process on alumina and the size 50.8 mm x 50.8 mm and the thickness of 0.63 mm. Every there exist several products which were designed for burying in substrate contained initially four identical test structures in a low temperature cofired ceramic tape (LTCC). To achieve high form of planar capacitors comprising electrode layers separated dielectric constants, substances must be used which are similar by two or three layers of dielectric. The electrodes had a in their structure to popular piezoelectric materials like PZT or diameter of 12 mm, the total thickness of dielectric film ranged BaTiO3, so they also show piezoelectric behaviour. The effect from 30 µm to 50 µm. After the last firing step (top electrode) of the piezoelectricity is well known for multilayer ceramic chip the samples were singulated as shown in Fig. 1. capacitors, manifesting itself as microphonics on one hand and as sound emission under switching conditions on the other. All layers of the test structure were separately printed, dried and fired; used materials and process parameters are given in In this work piezoelectric properties of several high-K Table I. It is known from literature that conductor pastes used dielectric pastes from ESL ElectroScience (now Ferro for building the capacitor stack can greatly influence relative Corporation) were investigated. The primary goal was to permittivity and piezoelectric response of the dielectric [1], [3]. determine if the substantial piezoelectric effect in the printed For our tests not only the recommended material combinations high-K dielectrics can be observed and, if applicable, to find the were used, as indicated in the table. necessary conditions for polarising the film (electric field strength, duration of the process and its temperature). The piezo effect can, on one hand, cause problems in printed capacitors TABLE I. THICK FILM PASTES USED FOR TEST STRUCTURES. with respect to microphonics and actuator action. On the other Dielectric Electrode Firing hand, it could prove sensible to use these printed films in Recommended Used Conditions piezoelectric components: advantages would be that they are 4113-H 9638 9635-G 930°C / 1 h readily available, have compatible electrode and sealant pastes 4117 9638 9635-G 930°C / 1 h and are long proven in production. 4163-N 9916 9912-K 850°C / 1 h 4212-C 9916, 9516, 8816 9516 850°C / 1 h In order to estimate whether applications as sensor or actuator films are possible, the aging rate of piezoelectric © IMAPS / EMPC 2017 1 European Microelectronics 10-13 September 2017, Warsaw, Poland Packaging Conference www.empc2017.pl , relatively high variability ([9], [10]) but it is suitable to quickly to the bending moment in the centre of the dielectric film. The � � � � characterise the samples. In our measurements, where the goal bending moment at is given by � �� �� �� �� � where � �� and�� �� denote�� �� piezoelectric�� �� � coefficients, was not to determine the exact piezoelectric coefficients but to find conditions for polarising the dielectric and to measure the �� are components�� �� of the stress�� tensor in the dielectric film, � � �� � time dependence of relaxation, this direct measurement of is the dielectric permittivity at constant stress and is electric� � �� ��� was absolutely sufficient. ��� � field strength. This equation was used to find the piezoelectric �� � � � � �� coefficients from the direct piezoelectric effect. �� � �� � �� ��� �⋅� A substantially better sensitivity and a higher signal-noise where denotes the vertical�� acceleration of the system due ratio than for the Berlincourt-like approach was achieved by a To determine the in-plane stress components and to oscillations of the platform (rms value), is the width of the direct measurement of response. This type of measurement �� � substrate� in direction. The outer beam fibre of the substrate as well as the ��electric field were held at zero� (“no allowed determining piezoelectric coefficients well below � � �� with thickness would experience stress in� direction clamping”� and “short-circuit” conditions respectively). The 1 pC/N, using experimental� setup presented in Fig. 4. Due to the experimental�� setup was very similar� to� the standard Berlincourt- � load and to the fixture, the oscillation of the shaker platform � � type measurement (Fig. 3), which relies on measurement of introduces a bending stress in the sample (about the axis), change in electric displacement due to the introduced change in resulting in the normal stress in the dielectric film (along the stress. The sample loaded by a spherical mass was put on the axis). Since stresses in and directions are not induced,� and � 6 ��� � �� � Fig. 1. Measurement sample with the test capacitor structure. shaker platform, which moved vertically with amplitude the electric field in the film is held at zero by the charge� Assuming same strains in the printed�� layer and in the outer and frequency . The acceleration of the platform ( amplifier, the piezoelectric� response� can be calculated from substrate fibre adjacent to it, the absolute value of the stress in III. PHYSICAL BACKGROUND AND EXPERIMENTAL SETUP , rms value) created a sinusoidal force 10 μm in (1) as: �� �� dielectric film can be calculated: addition to the� static40 Hz preload due to the weight of the sphere.� � � � �� A. Hysteresis Loops and Relative Permittivity Given0.446 m/s the mass of the sphere the forces� can be �� �� To acquire hysteresis P-E loops a modified Sawyer-Tower calculated: � �� circuit with numerical charge integration was used [4] (Fig. 2). � � �0.4 � � � �� � � � �� � �� � � � � 6� � This allowed measuring loops at frequency as low as 50 mHz. � � � � � � � � � �� � �� � � �� ��� �⋅ ⋅ � Compensation of the circuit was performed digitally; following The electric displacement �� is determined as the ratio of Here and � are the Young’s�� modulus�� values� for the �� effects were taken into account: (a) input offset voltage of the �� �� �� �� �� the generated charge to the electrode area; the stress in the film substrate and dielectric film respectively. For alumina � �� � � � 0.6� N � �� �� � �.14 � 10 N � � � acquisition card, which manifests itself as a linear rise (or fall) The coefficient was then determined as is found from the elastic beam�� theory (e.g. [11]) in a simplified �was taken� [12], the modulus for the dielectric layer of the calculated charge on the electrodes, (b) dielectric loss in ��� approach described below. It is assumed, that the printed was assumed to be based on literature values� �for� the material leading to a phase shift of the current in the shunt �� dielectric and electrodes layers do not influence the bending of � screen-printed340 GPa PZT layers [13], [14] and [15]. resistance. The charge offset (integration constant) was defined the alumina substrate but are deformed with the same strain as � ��� ��� �� � � 60 GPa from the symmetry of the ac signal. ��� � � � the outer substrate fibre. This assumption can be corroborated To investigate the variability of results and characterise the where stands for the rms value� �of�� the measured charge. by the geometry of the samples:
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