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Fast actuation speed, large-shape deformation and robust responsiveness are critical to synthetic soft actuators. A simultaneous optimization of all these aspects without trade-offs remains unresolved. Here we describe porous polymer actuators that bend in response to acetone vapour (24 kPa, 20 degrees C) at a speed of an order of magnitude faster than the state-of-the-art, coupled with a large-scale locomotion. They are meanwhile multi-responsive towards a variety of organic vapours in both the dry and wet states, thus distinctive from the traditional gel actuation systems that become inactive when dried. The actuator is easy-to-make and survives even after hydrothermal processing (200 degrees C, 24 h) and pressing-pressure (100 MPa) treatments. In addition, the beneficial responsiveness is transferable, being able to turn 'inert' objects into actuators through surface coating. This advanced actuator arises from the unique combination of porous morphology, gradient structure and the interaction between solvent molecules and actuator materials.
Dielectric elastomers (DE) are soft polymer materials exhibiting large deformations under electrostatic stress. When a prestretched elastomer is stuck to a flat plastic frame, a complex structure that can be used as an actuator (DEA) is formed due to self-organization and energy minimization. Here, such a DEA was equipped with a ferroelectret film. Ferroelectrets are internally charged polymer foams or void-containing polymer-film systems combining large piezoelectricity with mechanical flexibility and elastic compliance. In their dielectric spectra, ferroelectrets show piezoelectric resonances that can be used to analyze their electromechanical properties. The antiresonance frequencies ( ) of ferroelectret films not only are directly related to their geometric parameters, but also are sensitive to the boundary conditions during measurement. In this paper, a fluoroethylenepropylene (FEP) ferroelectret film with tubular void channels was glued to a plastic frame prior to the formation of self-organized minimum-energy DEA structure. The dielectric resonance spectrum (DRS) of the ferroelectret film was measured in-situ during the actuation of the DEA under applied voltage. It is found that the antiresonance frequency is a monotropic function of the bending angle of the actuator. Therefore, the actuation of DEAs can be used to modulate the of ferroelectrets, while the can also be taken for in-situ diagnosis and for precise control of the actuation of the DEA. Combination of DEAs and ferroelectrets brings a number of possibilities for application.
Laminated polymer-film systems with well-defined void structures were prepared from fluoroethylenepropylene (FEP) and polytetrafluoroethylene (PTFE) layers. First the PTFE films were patterned and then fusion-bonded with the FEP films. The laminates were subjected to either corona or contact charging in order to obtain the desired piezoelectricity. The build-up of the "macro-dipoles" in the laminated films was studied by recording the electric hysteresis loops. The resulting electro-mechanical properties were investigated by means of dielectric resonance spectroscopy (DRS) and direct measurements of the stress-strain relationship. Moreover, the thermal stability of the piezoelectric d (33) coefficient was investigated at elevated temperatures and via thermally stimulated discharge (TSD) current measurements in short circuit. For 150 mu m thick laminated films, consisting of one 25 mu m thick PTFE layer, two 12.5 mu m thick FEP layers, and a void of 100 mu m height, the critical voltage necessary for the build-up of the "macro-dipoles" in the inner voids was approximately 1400 V, which agrees with the value calculated from the Paschen Law. A quasi-static piezoelectric d (33) coefficient up to 300 pC/N was observed after corona charging. The mechanical properties of the film systems are highly anisotropic. At room temperature, the Young's moduli of the laminated film system are around 0.37 MPa in the thickness direction and 274 MPa in the lateral direction, respectively. Using these values, the theoretical shape anisotropy ratio of the void was calculated, which agrees well with experimental observation. Compared with films that do not exhibit structural regularity, the laminates showed improved thermal stability of the d (33) coefficients. The thermal stability of d (33) can be further improved by pre-aging. E.g., the reduction of the d (33) value in the sample pre-aged at 150A degrees C for 5 h was less than 5% after annealing for 30 h at a temperature of 90A degrees C.
We report a process for preparing polymer ferroelectrets by means of screen printing-a technology that is widely used for the two-dimensional patterning of printed layers. In order to produce polymer-film systems with cavities that are suitable for bipolar electric charging, a screen-printing paste is deposited through a screen with a pre-designed pattern onto the surface of a polymer electret film. Another such polymer film is placed on top of the printed pattern, and well-defined cavities are formed in-between. During heating and curing, the polymer films are tightly bonded to the patterned paste layer so that a stable three-layer system is obtained. In the present work, polycarbonate (PC) films have been employed as electret layers. Screen printing, curing and charging led to PC ferroelectret systems with a piezoelectric d (33) coefficient of about 28 pC/N that is stable up to 100 C-a similar to. Due to the rather soft patterned layer, d (33) strongly decreases already for static pressures of tens of kPa. The results demonstrate the suitability of screen printing for the preparation of ferroelectret systems.
Ferroelectrets have been fabricated from low-density polyethylene (LDPE) films by means of a template-based lamination. The temperature dependence of the piezoelectric d(33) coefficient has been investigated. It was found that low-density polyethylene ferroelectrets have rather low thermal stability with the piezoelectric coefficient decaying almost to zero already at 100 degrees C. This behavior is attributed to the poor electret properties of the polyethylene films used for the fabrication of the ferroelectrets. In order to improve the charge trapping and the thermal stability of electret charge and piezoelectricity, LDPE ferroelectrets were treated with orthophosphoric acid. The treatment resulted in considerable improvements of the charge stability in LDPE films and in ferroelectret systems made from them. For example, the charge and piezoelectric-coefficient decay curves shifted to higher temperatures by 60 K and 40 K, respectively. It is shown that the decay of the piezoelectric coefficient in LDPE ferroelectrets is governed by the relaxation of less stable positive charges. The treatment also leads to noticeable changes in the chemical composition of the LDPE surface. Infrared spectroscopy reveals absorption bands attributed to phosphorus-containing structures, while scanning electron microscopy shows new island-like structures, 50-200 nm in diameter, on the modified surface.
Cellular polypropylene (PP) ferroelectrets combine a large piezoelectricity with mechanical flexibility and elastic compliance. Their charging process represents a series of dielectric barrier discharges (DBDs) that generate a cold plasma with numerous active species and thus modify the inner polymer surfaces of the foam cells. Both the threshold for the onset of DBDs and the piezoelectricity of ferroelectrets are sensitive to repeated DBDs in the voids. It is found that the threshold voltage is approximately halved and the charging efficiency is clearly improved after only 10(3) DBD cycles. However, plasma modification of the inner surfaces from repeated DBDs deteriorates the chargeability of the voids, leading to a significant reduction of the piezoelectricity in ferroelectrets. After a significant waiting period, the chargeability of previously fatigued voids shows a partial recovery. The plasma modification is, however, detrimental to the stability of the deposited charges and thus also of the macroscopic dipoles and of the piezoelectricity. Fatigue from only 10(3) DBD cycles already results in significantly less stable piezoelectricity in cellular PP ferroelectrets. The fatigue rate as a function of the number of voltage cycles follows a stretched exponential. Fatigue from repeated DBDs can be avoided if most of the gas molecules inside the voids are removed via a suitable evacuation process.
Polarization and Hysteresis in Tubular-Channel Fluoroethylenepropylene-Copolymer Ferroelectrets
(2014)
Polarization-vs.-applied-voltage hysteresis curves are recorded on tubular-channel fluoroethylene-propylene (FEP) copolymer ferroelectrets by means of a modified Sawyer-Tower circuit. Dielectric barrier discharges (DBDs) inside the cavities are triggered when the applied voltage is sufficiently high. During the DBDs, the cavities become man-made macroscopic dipoles which build up an effective polarization in the ferroelectret. Therefore, a phenomenological hysteresis curve is observed. From the hysteresis loop, the remanent polarization and the coercive field can be determined. Furthermore, the polarization can be related to the respective piezoelectric coefficient of the ferroelectret. The proposed method is easy to implement and is useful for characterization, further development and optimization of ferro- or piezoelectrets.
The influence of the temperature in the gas-filled cavities on the charging process of ferroelectret film systems has been studied in hysteresis measurements. The threshold voltage and the effective polarization of the ferroelectrets were determined as functions of the charging temperature TP. With increasing TP, the threshold voltage for triggering dielectric barrier discharges in ferroelectrets decreases. Thus, increasing the temperature facilitates the charging of ferroelectrets. However, a lower threshold voltage reduces the attainable remanent polarization because back discharges occur at lower charge levels, as soon as the charging voltage is turned off. The results are discussed in view of Paschen's law for electrical breakdown, taking into account the respective gas temperature and a simplified model for ferroelectrets. Our results indicate that the thermal poling scheme widely used for conventional ferroelectrics is also useful for electrically charging ferroelectrets.
Ferroelectrets (sometimes also called piezoelectrets) are relatively new members of the family of piezo-, pyro-, and ferroelectric materials.1–5 As their name indicates, ferroelectrets are space-charge electrets that show ferroic behavior. They are non-uniform electret materials or materials systems with electrically charged internal cavities. As space-charge electrets, ferroelectrets usually do not contain any molecular dipoles. However, the cavities inside the material can be turned into macroscopic dipoles through a series of micro-plasma discharges at high electric fields, so-called dielectric barrier discharges (DBDs).6–8 The gas inside the cavities is ionized when the internal electric field exceeds the threshold for electrical breakdown, generating charges of both polarities.9 The positive and negative charges travel in opposite directions, and are eventually trapped at the internal top and bottom surfaces of the cavities, respectively. After charging, the cavities may be regarded as macroscopic dipoles that can be switched by reversing the applied voltage.
An electric-polarization-vs.-electric-field (P(E)) hysteresis is considered as an essential criterion for ferroelectricity. P(E)-hysteresis curves are usually characterized by the spontaneous polarization, the coercive field, and the remanent polarization. Recently, we have demonstrated P(E)-hysteresis loops on two different types of ferroelectrets, namely, cellular polypropylene ferroelectrets and tubular-channel fluoroethylene-polypropylene copolymer ferroelectrets.10,11 The P(E)-hysteresis loops not only prove the ferroic behavior of ferroelectrets, but also allow us to determine such parameters as the coercive field and the remanent polarization.
It is widely accepted that Paschen breakdown is the underlying mechanism for the inception of DBDs in ferroelectrets.12–14 On this basis, the charging behavior and the resulting piezoelectricity of ferroelectrets in different gases at various pressures have been studied.15–17 Paschen's law describes the conditions for electrical breakdown in a gas at a constant temperature (usually room temperature), and it needs to be modified for gas breakdown at other temperatures. The temperature stability of the piezoelectricity in ferroelectrets after charging at elevated temperatures was investigated by several researchers.18–21 Recently, a preliminary report about the effects of the charging temperature on the hysteresis loops in ferroelectrets has been presented.22
In this letter, the influence of the gas temperature on the charging of ferroelectret systems is investigated in more detail by means of quasi-ferroelectric hysteresis-loop measurements. Teflon™ fluoroethylenepropylene (FEP) copolymer samples with tubular channels were prepared via thermal lamination as described previously.23 To this end, two FEP films with a thickness of 50 μm each were laminated at 300 ° C
around a 100 μm thick polytetrafluoroethylene (PTFE) template (total area 35 mm × 45 mm) that contains parallel rectangular openings (area 1.5 mm × 40 mm each). After lamination, the template was removed, which results in an FEP film system with open tubular channels. The samples were metallized on both surfaces with aluminum electrodes of 20 mm diameter.
P(E)-hysteresis loops were obtained with a modified Sawyer–Tower (ST) circuit.10,11 A high-voltage (HV) capacitor C1 (3 nF) and a large standard capacitor Cm (1 μF) were connected in series with the sample. A bipolar sinusoidal voltage with a frequency of 10 mHz was applied from an HV power supply (FUG HCB 7-6500) controlled by an arbitrary-waveform generator (HP 33120a). The voltage Vout
on Cm is measured by means of an electrometer (HP 3458a), and the charge flowing through the circuit is determined as Q(t)=CmVout(t)
. The experiments were carried out at isothermal conditions in a Novocontrol® Quatro cryosystem.
With the modified ST circuit, Q–V loops have been measured on a tubular-channel FEP ferroelectret system at different temperatures. The sample capacitance of about 34.5 pF is determined by a linear fit of the initial part of the Q–V curve recorded at 20 °C
, where the voltage has been raised up from zero on a fresh sample. The hysteresis loops are obtained from the Q–V curves by subtracting the contribution that results from charging of the sample capacitance.10 Figure 1 shows the hysteresis loops of the sample at −100, 0, and +100 ° C, respectively. According to previous theoretical and experimental studies,24,25 the length of each of the horizontal sides of the parallelogram-like hysteresis loops is given by 2Vth where Vth is the threshold voltage. As the charging temperature decreases, the hysteresis loop becomes wider and less high, i.e., the threshold voltage increases, while the polarization at maximum voltage decreases.
Spectroscopic study of dielectric barrier discharges in cellular polypropylene ferroelectrets
(2007)
The transient light emission from the dielectric barrier discharges (DBDs) in cellular polypropylene ferroelectrets subjected to high electric poling fields was spectroscopically measured. The spectrum shows strong emission from the second positive system of molecular nitrogen, N-2(C (3)Pi(u))-> N-2(B (3)Pi(g)), and the first negative system of N-2(+), N-2(+)(B (2)Sigma(+)(u))-> N-2(+)(X (2)Sigma(+)(g)), consistent with a DBD in air. When a dc voltage is applied stepwise to the ferroelectret film, light emission starts above a threshold, coinciding with the threshold voltage in obtaining piezoelectricity. From selected vibronic band strength ratios, the electric field in the discharge was determined and found to agree with Townsend breakdown.