• Smart Structures and Systems
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• v.12 no.1
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• pp.55-71
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• 2013

Structural health monitoring (SHM) is vital for detecting the onset of damage and for preventing catastrophic failure of civil infrastructure systems. In particular, piezoelectric transducers have the ability to excite and actively interrogate structures (e.g., using surface waves) while measuring their response for sensing and damage detection. In fact, piezoelectric transducers such as lead zirconate titanate (PZT) and poly(vinylidene fluoride) (PVDF) have been used for various laboratory/field tests and possess significant advantages as compared to visual inspection and vibration-based methods, to name a few. However, PZTs are inherently brittle, and PVDF films do not possess high piezoelectricity, thereby limiting each of these devices to certain specific applications. The objective of this study is to design, characterize, and validate piezoelectric nanocomposites consisting of zinc oxide (ZnO) nanoparticles assembled in a PVDF copolymer matrix for sensing and SHM applications. These films provide greater mechanical flexibility as compared to PZTs, yet possess enhanced piezoelectricity as compared to pristine PVDF copolymers. This study started with spin coating dispersed ZnO- and PVDF-TrFE-based solutions to fabricate the piezoelectric nanocomposites. The concentration of ZnO nanoparticles was varied from 0 to 20 wt.% (in 5 % increments) to determine their influence on bulk film piezoelectricity. Second, their electric polarization responses were obtained for quantifying thin film remnant polarization, which is directly correlated to piezoelectricity. Based on these results, the films were poled (at 50 $MV-m^{-1}$) to permanently align their electrical domains and to enhance their bulk film piezoelectricity. Then, a series of hammer impact tests were conducted, and the voltage generated by poled ZnO-based thin films was compared to commercially poled PVDF copolymer thin films. The hammer impact tests showed comparable results between the prototype and commercial samples, and increasing ZnO content provided enhanced piezoelectric performance. Lastly, the films were further validated for sensing using different energy levels of hammer impact, different distances between the impact locations and the film electrodes, and cantilever free vibration testing for dynamic strain sensing.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2006.06a
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• pp.169-170
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• 2006

In this study, ultra thin films of ferroelectric vinylidene fluoride-trifluoroethylene (VF2-TrFE) copolymer were fabricated on degenerated Si (n+, $0.002\;{\Omega}{\cdot}cm$) using by spin coating method. A 1~5 wt% diluted solution of purified vinylidene fluoride-trifluoroethylene (VF2:TrFE=70:30) in a dimethylformamide (DMF) solvent were prepared and deposited on silicon wafers at a spin rate of 2000~5000rpm for 30 seconds. After annealing in a vacuum ambient at $200^{\circ}C$ for 60 min, upper gold electrodes were deposited by vacuum evaporation for electrical measurement. X-ray diffraction results showed that the VF2-TrFE films on Si substrates had $\beta$-phase of copolymer structures. The capacitance on $n^+$-Si(100) wafer showed hysteresis behavior like a butterfly shape and this result indicates clearly that the dielectric films have ferroelectric properties. The typical measured remnant polarization (2Pr) and coercive filed (EC) values measured using a computer controlled a RT-66A standardized ferroelectric test system (Radiant Technologies) were about $0.54\;C/cm^2$ and 172 kV/cm, respectively, in an applied electric field of ${\pm}0.75\;MV/cm$.

• Proceedings of the KIEE Conference
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• 1996.07c
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• pp.1472-1475
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• 1996

D-E hysteresis loops have been measured for the 65/35 mole % copolymer of vinylidene fluoride and trifIuoroethyIene over wide temperature range. The results were analyzed and discussed. The remanent polarization and the coercive field at room termperature were estimated to be 75 $mC/m^3$ and 55 MV/m respectively. D-E hysteresis loops were observed even below the glass transiation temperature$-20^{\circ}C$) and the remanent polarization and the coercive field were larger than larger, as the temperature lower. It seems that the remanent polarization and the coercive field depend on the amorphous region as well as crystalline region in this copolymer. And the ferroelectric-to-paraelectric phase transition was observed at $90^{\circ}C$ on heating and $80^{\circ}C$ on cooling. Double hysteresis loops were observed at the temperature($85^{\circ}C$) of paraelectric phase.

• Electrical & Electronic Materials
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• v.10 no.2
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• pp.156-165
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• 1997

D-E hysteresis loops have been measured for the 65/35 mole % copolymer of vinylidene fluoride and trifluoroethylene over wide temperature range. The remanent polarization and the coercive field at room temperature were estimated to be 75 mC/m$^{2}$ and 55 MV/m respectively. D-E hysteresis loops were observed even below the glass transition temperature(-20.deg. C) and the remanent polarization and the coercive field were larger, as the temperature lower. It seems that the remanent polarization and the coercive field depend on the amorphous region as well as crystalline region in this copolymer. And the ferroelectric-to-paraelectric phase transition was observed at 90.deg. C on heating and 80'C on cooling. Double hysteresis loops were observed at the temperature(85.deg. C) of paraelectric phase.

• Membrane Journal
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• v.17 no.4
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• pp.359-368
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• 2007

The copolymer membranes, poly(vinylidene fluoride-hexafluoropropylene) (PVdF-HFP) were prepared by phase inversion method using as an additive with N,N-dimethylformamid as a solvent. The pores are generated during the solvent and non-solvent exchange process in the coagulation bath filled with non-solvent (distilled water). The highest porosity of the membrane was 60%. The surface and cross-section of the membranes was observed with a scanning electron microscopy (SEM). The mechanical property of the membrane was determined by using an universal testing machine (UTM). Tensile strength of measured membranes is presented the maximum 6.57 MPa at 30 wt% of PVdF-HFP.

• Korean Membrane Journal
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• v.10 no.1
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• pp.20-25
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• 2008

Proton conducting composite membranes were prepared by solution blending of poly(vinylidene fluoride-co-chlorotrifluoroethylene)-graft-poly(sulfopropyl methacrylate) (P(VDF-CTFE)-g-PSPMA) graft copolymer and heteropolyacid (HPA). The P(VDF-CTFE)-g-PSPMA graft copolymer was synthesized by atom transfer radical polymerization (ATRP) using direct initiation of the secondary chlorines of P(VDF-CTFE). FT-IR spectroscopy revealed that HPA nanoparticles were incorporated into the graft copolymer via hydrogen bonding interactions. The water uptake of membranes continuously decreased with increasing HP A concentration up to 45wt%, after which it slightly increased. It is presumably due to the decrease in number of water absorption sites due to hydrogen bonding interaction between the HP A particles and the polymer matrix. The proton conductivity of membranes increased with increasing HPA concentration up to 45wt%, resulting from both the intrinsic conductivity of HP A particles and the enhanced acidity of the sulfonic acid of the graft copolymer.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.11a
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• pp.115-116
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• 2008

The ferroelectric vinylidene fluoride-trifluoroethylene ($VF_2$-TrFE) and $Al_2O_3$ passivation layer for the Metal/Insulator/Ferroelectric/Semiconductor (MIFS) structure were deposited using spin coating and remote plasma atomic layer deposition (RPALD), respectively. A 2.5 ~ 3 wt % diluted solution of purified vinylidene fluoride-trifluoroethylene ($VF_2$: TrFE=70:30) in a DMF solution were prepared and deposited on silicon wafer at a optimized spin speed. After annealing in a vacuum ambient at 150 ~ $200^{\circ}C$ for 60 min, upper insulator layer were deposited at temperature ranging from 100 ~ $150^{\circ}C$ by RPALD. We described electrical and structural properties of MIFS fabricated by spin coating and RPALD methods.

• Bulletin of the Korean Chemical Society
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• v.32 no.7
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• pp.2345-2350
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• 2011

Variable temperature high-resolution $^{19}F$ magic angle spinning (MAS) solid-state NMR spectroscopy was used to characterize fluorocarbon (FKM) rubbers. The high-resolution spectra of copolymers made from two monomers, vinylidene fluoride and hexafluoropropene, and terpolymers composed of vinylidene fluoride, hexafluoropropene, and tetrafluoroethylene, were obtained using MAS speeds of up to 18 kHz combined with high temperatures of up to 200 $^{\circ}C$ at a magnetic field strength of 9.4 Tesla. From these high resolution solid-state NMR spectra, we were able to assign the spectral peaks and differentiate the copolymer FKM from the terpolymer FKM. We also determined quantitatively the monomer compositions of each FKM rubber.

• Polymer(Korea)
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• v.37 no.1
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• pp.74-79
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• 2013

Polyvinylidene fluoride (PVDF) and its copolymer with hexafluoropropylene (HFP) were successfully prepared from free radical solution polymerizations using diisopropyl peroxidicarbonate (DIPPDC) in the presence of 1,1,2-trichlorotrifluoroethane (R-113). The reactivity ratios of VDF and HFP were estimated as$r_{VDF}=2.06{\pm}0.03$ and $r_{HFP}{\approx}0$. This result indicates that HFP cannot undergo self propagation. The weight-average molecular weight and molecular weight distribution of copolymers were found to decrease with increasing HFP content. The melting temperature of copolymers linearly decreased with the increase of HFP content because of the introduction of HFP. Moreover, no melting peak was observed for the copolymers with high HFP content. The glass transition temperature of copolymers gradually increased with the increase of HFP content due to the restricted flexibility of the polymer chains.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.11a
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• pp.85-86
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• 2007

A poly(vinylidene fluoride-trifluoroethyene) (P(VDF-TrFE)) copolymer thin film having ${\beta}$ phase was prepared by sol-gel method. The electrical properties of the film were studied to evaluate the possibility for appling to a ferroelectric random access memory. In order to characterize its electrical properties, we produced a MFS (metal-ferroelectric-semiconductor) structure by evaporation of Au electrodes. The C-V (capacitance-voltage) measurement revealed that the Au/P(VDF-TrFE)/Si structure with a 4 wt% film had a memory window width of about 0.5V for a bias voltage sweep of 1V.