Physical characteristics of polyimide films for flexible sensors

Physical characteristics of polyimide films, including optical, micro/nano mechanical, and thermophysical characteristics were investigated using a photometric, a nanoindentation, and a thermomechanical analyzer for applications in flexible sensors. Experimental results show that UV light cannot transmit into the polyimide films. The transmittances, with a maximum of about 86%, at VIS and near IR lights decrease with increasing PI film thicknesses. The mechanical characteristics were determined using tensile, bending moment, and nanoindentation testing. The stress–strain curve approximated bilinear characteristics, the load–unload bending moment exhibited hysteresis, and nanoindentation generated elastic energy dissipation in the loading–unloading region. Nanoindentation showed an almost uniform hardness and a reduced Young’s modulus of about 0.181±0.03 and 3.21±0.06 GPa, respectively, when the penetrating depth was more than about 2 μm. Thermophysical characteristics were greatly influenced on 8.3 and 25 μm specimens due to the higher relaxation of thin PI films. The thermal expansion remained steady when the thickness was over 50 μm. The results show that PI films have potential in flexible sensing and higher temperature fabrication.     

Micromechanical properties of carbon–silica aerogel composites

Materials’ endurance to mechanical stress is desirable from a technological point of view. In particular, in the case of silica aerogels, an improvement of the material elasticity is needed for some applications. Carbon–silica aerogel composites have been obtained and their mechanical properties, Young’s modulus, elastic parameter and hardness, have been evaluated with a dynamical, non-destructive microindentation technique. Large changes are found in Young’s modulus when only a small amount of carbon is added. This is clearly shown in the shape of the indentation curves as well as in the increase of the elastic parameter value, which evaluates the percentage of elasticity versus plasticity. Young’s modulus values obtained for carbon–silica aerogels show a similar variation with the carbon mass fraction to that predicted by a commonly used model for composite materials. The measured hardness values corresponding to the total elastoplastic deformation do not show such a prominent dependency on the carbon mass fraction as the elastic parameter and Young’s modulus do and they are similar to those measured for the pure-silica aerogel. Received: 18 May 2001 / Accepted: 30 July 2001 / Published online: 30 October 2001     

Preparation and characterization of anhydrous polymer electrolyte membranes based on poly(vinyl alcohol-<Emphasis Type="Italic">co</Emphasis>-ethylene) copolymer

Anhydrous polymer electrolyte membranes with cross-linked structure have been prepared based on poly(vinyl alcohol-co-ethylene) (PVA-co-PE) copolymer. The PVA units of copolymer served to induce thermal cross-linking with 4,5-imidazole dicarboxylic acid (IDA) via esterification while PE units controlled the membrane swelling and the mechanical properties of films. Upon doping with phosphoric acid (PA, H₃PO₄) to form imidazole-PA complexes, the proton conductivity of membranes continuously increased with increasing PA content. As a result, proton conductivity reached 0.01 S/cm at 100 °C under anhydrous conditions. X-ray diffraction analysis revealed that both the d-spacing and crystalline peak of membranes were reduced upon introduction of IDA/PA due to the cross-linking effect. The PVA-co-PE/IDA/PA membranes exhibited good mechanical properties, e.g., 150 MPa of Young’s modulus, as determined by a universal testing machine. Thermal gravimetric analysis also represented that the thermal stability of membranes was increased up to 200 °C upon introduction of IDA/PA.     

Young’s modulus and density of nanocrystalline cubic boron nitride films determined by dispersion of surface acoustic waves

Cubic boron nitride (c-BN) films of 200–420 nm thickness and high phase purity were deposited on silicon (100) substrates by ion-assisted pulsed laser deposition (IA PLD)from a boron nitride target using a KrF-excimer laser, and by plasma-enhanced physical vapor deposition (PE PVD)with a hollow-cathode arc evaporation device. In order to improve the c-BNfilm adhesion, hexagonal boron nitride (h-BN) films with 25–50 nm thickness were used as buffer layers. The density and Young’s modulus of the c-BNfilms were obtained by investigating the dispersion of surface acoustic waves. In data analysis a two-layer model was applied in order to take the influence of the h-BNlayer into consideration. The values for the density vary from 2.95±0.25 g/cm³to 3.35±0.3 g/cm³, and those for the Young’s modulus from 420±40 GPa to 505±30 GPa. The results are compared with literature values reported for nanocrystalline films, polycrystalline disks and single crystal c-BN. Received: 26 March 2001 / Accepted: 29 March 2001 / Published online: 25 July 2001     

Pulsed holmium laser ablation of tissue phantoms: correlation between bubble formation and acoustic transients

5 Pa served as tissue phantoms to evaluate such effects. Holmium laser pulses (wavelength: 2.12 μm, duration: 180 μs FWHM), were delivered through 400 and 600 μm diameter optical fibers inserted into cubes of clear gel. Bubble effects were investigated using simultaneous flash micro-videography and pressure recording for radiant exposures of 20–382 J/cm². Bubble formation and bubble collapse induced pressure transients were observed regardless of phantom stiffness. Bubbles of up to 4.2 mm in length were observed in gels with a Young’s modulus of 2.9×10⁵ Pa at a pulse energy of 650 mJ. An increase of Young’s modulus (reduction in water content) led to a monotonic reduction of bubble size. In the softest gels, bubble dimensions exceeded those observed in water. Pressure amplitudes at 3 mm decreased from 100±14 bars to 17±6 bars with increasing Young’s modulus over the studied range. Theoretical analysis suggested a major influence on bubble dynamics of the mass and energy transfer through the bubble boundary. Received: 26 August 1996/Revised version: 10 February 1997     

Electrical properties and photoconductivity of polyaniline/sulfonated poly(arylene ether sulfone) composite films

Temperature dependent electrical conductivity of the polyaniline-sulfonated poly(arylene ether sulfone) with 35 mol percent sulfonation (PANI-BPS35) composite films were investigated in the temperature range of 80–380 K. These composite films showed semiconductor behavior with the exponential variation of inverse temperature dependence of electrical conductivity. Calculated Mott’s parameters showed that variable range hopping mechanism is the dominant transport mechanism for the carriers in low temperature region. Photoconductivity of the PANI-BPS35 composite films having 10, 20, and 40 weight percent conductive filler under various illumination intensities was also studied. Photocurrent of the composite films increased with increasing both polyaniline weight fraction and temperature. Finally, the effect of doping on both electrical conductivity and the photoconductivity of the composite films was investigated.     

A Monte Carlo and continuum study of mechanical properties of nanoparticle based films

A combination Monte Carlo and equivalent-continuum simulation approach was used to investigate the structure-mechanical property relationships of titania nanoparticle deposits. Films of titania composed of nanoparticle aggregates were simulated using a Monte Carlo approach with diffusion-limited aggregation. Each aggregate in the simulation is fractal-like and random in structure. In the film structure, it is assumed that bond strength is a function of distance with two limiting values for the bond strengths: one representing the strong chemical bond between the particles at closest proximity in the aggregate and the other representing the weak van der Waals bond between particles from different aggregates. The Young’s modulus of the film is estimated using an equivalent-continuum modeling approach, and the influences of particle diameter (5–100 nm) and aggregate size (3–400 particles per aggregate) on predicted Young’s modulus are investigated. The Young’s modulus is observed to increase with a decrease in primary particle size and is independent of the size of the aggregates deposited. Decreasing porosity resulted in an increase in Young’s modulus as expected from results reported previously in the literature.     

Investigations on Fe doped polyvinyl alcohol films with and without gamma (γ)-irradiation

This paper deals with the preparation of pure and ferric chloride (FeCl₃) doped polyvinyl alcohol (PVA) films by solution casting method. Optical and electrical properties were systematically investigated. We have found the decrease in optical band gap energy of PVA films on doping FeCl₃. The optical band gap energy values in the present work are found to be 3.10 eV for pure PVA, 2 eV for PVA:Fe³⁺ (5 mol%), 1.91 eV for PVA:Fe³⁺(15 mol%) and 1.8 eV for PVA:Fe³⁺(25 mol%). Direct current electrical conductivity (σ) of pure, FeCl₃ doped PVA films in the temperature range 70-127 °C has been studied. At 387 K dc electrical conductivity of pure PVA film is 5.5795 μ Ω⁻¹ cm⁻¹, PVA:Fe³⁺ (5 mol%) film is 10.0936 μ Ω⁻¹ cm⁻¹ and γ-Irradiated PVA:Fe³⁺ (5 mol%) film for 900 CGY/min is 22.1950 μ Ω⁻¹ cm⁻¹. The result reveals the enhancement of the electrical conductivity with γ-irradiation. FT-IR study signifies the intermolecular hydrogen bonding between Fe³⁺ ions of FeCl₃ with OH group of PVA.     

Structural and electrical properties of pure and H<Subscript>2</Subscript>SO<Subscript>4</Subscript> doped (PVA)<Subscript>0.7</Subscript>(NaI)<Subscript>0.3</Subscript> solid polymer electrolyte

Solid polymer electrolytes (SPE) based on poly-(vinyl alcohol) (PVA)_0.7 and sodium iodide (NaI)_0.3 complexed with sulfuric acid (SA) at different concentrations were prepared using solution casting technique. The structural properties of these electrolyte films were examined by X-ray diffraction (XRD) studies. The XRD data revealed that sulfuric acid disrupt the semi-crystalline nature of (PVA)_0.7(NaI)_0.3 and convert it into an amorphous phase. The proton conductivity and impedance of the electrolyte were studied with changing sulfuric acid concentration from 0 to 5.1 mol/liter (M). The highest conductivity of (PVA)_0.7(NaI)_0.3 matrix at room temperature was 10⁻⁵ S cm⁻¹ and this increased to 10⁻³ S cm⁻¹ with doping by 5.1 M sulfuric acid. The electrical conductivity (σ) and dielectric permittivity (ε′) of the solid polymer electrolyte in frequency range (500 Hz–1 MHz) and temperature range (300–400) K were carried out. The electrolyte with the highest electrical conductivity was used in the fabrication of a sodium battery with the configuration Na/SPE/MnO₂. The fabricated cells give open circuit voltage of 3.34 V and have an internal resistance of 4.5 kΩ.     

Application of scanning force microscopy in nanotube science

Recent developments in the application of scanning force microscopy in nanotube science are reviewed. The non-destructive character of this technique allows the structural characterisation of (chemically modified) single- and multi-wall nanotubes deposited on substrates for further investigations such as electrical transport measurements. Furthermore, SFM is now an established tool for manipulation of nanotubes, which allows position control and determination of elastic constants such as the Young’s modulus. Finally it is shown that very sharp and stable probes for scanning force microscopy can be made from nanotubes due to their excellent stability and aspect ratio. Received: 17 May 1999 / Accepted: 18 May 1999 / Published online: 29 July 1999     

Transparence and electrical properties of ZnO-based multilayer electrode

Three-layered ZnO/Ag–Ti/ZnO structures were prepared using both the sol-gel technique and DC magnetron sputtering. This study focuses on the electrical and optical properties of the ZnO/Ag–Ti/ZnO multilayers with various thicknesses of the Ag–Ti layer. The ZnO thin film prepared by the sol–gel method was dried at 300°C for 3 minutes, and a fixed thickness of 20 nm was obtained. The thickness of the Ag–Ti thin film was controlled by varying the sputtering time. The Ag–Ti layer substantially reduced the electrical resistivity of the sol–gel-sprayed ZnO thin films. The sheet resistance of the Ag–Ti layer decreased dramatically and then became steady beyond a sputtering time of 60 s. The sputtering time of Ag–Ti thin film deposition was determined to be 60 s, taking into account the optical transmittance. Consequently, the transmittance of the ZnO/Ag–Ti/ZnO multilayer films was 71% at 550 nm and 60% at 350 nm. The sheet resistance was 4.2 Ω/sq.     

Ni-MH battery based on plasticized alkaline solid polymer electrolytes

Solid-state nickel metal hydride cells were fabricated using plasticized alkaline solid polymer electrolytes (ASPE) prepared from polyvinyl alcohol (PVA), potassium hydroxide (KOH), alumina (α-Al₂O₃), and propylene carbonate (PC). The ASPE film with PVA/KOH/α-Al₂O₃/PC/H₂O weight ratio of 1.00:0.67:0.09:2.64:1.32 and conductivity of (6.6 ± 1.7) × 10⁻⁴ S cm⁻¹ was used in fabrication of the electrochemical cells. To investigate the electrochemical properties of the plasticized ASPE, cells with the configuration Mg₂Ni/plasticized ASPE/Ni(OH)₂ were fabricated. At the eighth cycle with a current drain of 0.1 mA and plateau voltage of ∼1.1 V, the discharge lasted for 14 h before the cell was considered to have failed. The failure mode of the cell was due to the formation of thin Mg(OH)₂ insulating layers.     

Elasticity and polarization of Ga<Subscript>x</Subscript>Al<Subscript>1-x</Subscript>N alloys subjected to uniaxial and biaxial compression

Elasticity and polarization of Ga_xAl_1-xN alloys subjected to uniaxial and homogeneous biaxial compression are calculated using first-principles methods. The uniaxial compression along the c-axis reduces Young’s modulus along the c-axis, and enhances bulk modulus and total polarization, whereas the biaxial compression in the plane perpendicular to the c-axis enhances bulk and Young’s moduli. It is also found that when the in-plane biaxial compression is applied by constraining the a-axis lattice constant to that of AlN, the bulk and Young’s moduli dramatically increase with increasing Ga concentration, and the total polarization could be suppressed, even annihilated, and finally enhanced by controlling Ga concentration.     

Fluoride-doped MWCNT/Si3N4 composite with improved mechanical and structural properties

The addition of carbon nanotubes (CNT) in ceramic composites has stimulated a substantial interest due to their high mechanical, thermal and electrical properties. This approach used fluoride additives (AlF₃ and MgF₂) to prepare multi-walled carbon nanotubes/silicon nitride (MWCNT/Si₃N₄) composite densified at 1700 °C for 1 h by hot press (HP) sintering. The microstructural analyses of MWCNT/Si₃N₄ composites indicate that the fluoride additives have substantially improved densification and the transformation of α-Si₃N₄ to β-Si₃N₄. As observed, the mechanical properties, i.e. flexural strength, fracture toughness, Young's modulus and hardness of MWCNT/Si₃N₄ composites are improved with an increasing concentration of MWCNT. These results attributed to the highly dense composites, strong interfacial interaction and the pull-out mechanism of MWCNT and β-Si₃N₄. The maximum values of fracture toughness flexural strength, Young's modulus, and hardness were 12.76 ± 1.15 MPa.m^0.5, 883 ±46 MPa, 260 ±9 GPa, and 26.4 ± 1.3 GPa, respectively. The improved mechanical properties also ascribed to the synergistic strengthening and toughening influence of MWCNT and β-Si₃N₄.     

Amplitude dependence of the internal friction and Young’s modulus defect of polycrystalline indium

The dependences of the internal friction and the Young’s modulus defect of polycrystalline indium on the oscillatory strain amplitude have been studied over a wide range of temperatures (7–320 K) and oscillatory strain amplitudes (10⁻⁷−3.5 × 10⁻⁴) at oscillatory loading frequencies of about 100 kHz. It has been revealed that the amplitude dependences of the internal friction and the Young’s modulus defect include stages associated with the interaction of dislocations with point defects and the interdislocation interaction. The temperature range characterized by the formation of point-defect atmospheres (the Cottrell atmospheres) near dislocations in indium has been determined.     

Li ion conduction in TiO2 filled polyvinylidenefluoride-co-hexafluoropropylene based novel nanocomposite polymer electrolyte membranes with LiDFOB

This paper describes, nanocomposite polymer electrolyte (NCPE) based on polyvinylidenefluoride-co-hexafluoropropylene (PVdF-HFP), which comprises the novel lithium difluoro(oxalato)borate (LiDFOB). Ehtylene carbonate (EC) and diethyl carbonate (DEC) mixture was used as gelling agent and nanoparticulate TiO₂ used as filler. The NCPE membranes were subjected to a.c. impedance, tensile strength, Raman studies, TG/DTA and morphological studies. 5 wt% TiO₂ comprising membranes exhibited enhanced conductivity of 0.56 mS cm⁻¹and the Young’s modulus was increased from 1.32 to 2.74 MPa. The structural change of α to β phase was confirmed by Raman studies. The thermal stability of the NCPE membrane is found to be 130 °C. Calculation of activation energy and synthesis of LiDFOB has also been presented.     

Electrical properties and electromechanical responses of acrylic elastomers and styrene copolymers: effect of temperature

The electrical properties and electromechanical responses of acrylic elastomers and styrene copolymers were investigated towards electroactive applications such as artificial muscle and/or MEMS (micro-electro-mechanical systems) devices. The effect of temperature, between 300 and 370 K, on electrical conductivity, dielectric constant, storage and loss moduli (G’ and G”), storage modulus response (ΔG’_2 kV/mm), and the storage modulus sensitivity (ΔG’_2 kV/mm/G’₀) of acrylic elastomers and styrene copolymers were investigated under applied electric field strengths varying from 0 to 2 kV/mm. The acrylic elastomers (AR70, AR71, and AR72) possess linearly positive storage modulus responses or sensitivities with increasing temperature and dielectric constant. On the other hand, the styrene copolymers (SAR, SBS, and SIS) attain the maximum storage modulus responses or sensitivities at the glass-transition temperature of the hard segments. PACS  77.22.-d; 82.35.Lr; 83.60.Np; 83.80.Va; 91.60.Ki     

Study of the formation kinetics of Metastable phases in quenched Al-Mg-Si Alloys

The results of the experimental study of the formation kinetics of metastable phases during decomposition of supersaturated solid solutions of quenched Al-Mg-Si alloys are presented. The process has been studied by measuring the electrical conductivity at low temperatures (18–85°C) and by measuring the Young’s modulus using the acoustic method in the temperature range 120–220°C. The method of measuring the Young’s modulus is characterized by a high precision and has made it possible to distinguish between the successive stages of the decomposition due to the formation of Guinier-Preston zones, particles of the pre-β″/β″ and β′-phases. The effective activation energies have been calculated using the obtained data on the characteristic durations of the stages of the process at different temperatures. It has been shown that the activation energy of the formation and evolution of particles in the β″-phase is considerably lower than the activation energy of diffusion of alloying element atoms at equilibrium conditions, which is caused by the effect of long-lived quenching vacancies. This energy is close to the activation energy of migration of the ν + Mg complex and, according to the obtained results, is equal to 0.58 eV.     

Improved piezoelectric properties of cellular polypropylene ferroelectrets by chemical modification

To improve the thermal stability of piezoelectricity of polypropylene (PP) ferroelectrets, chemical modification of the cellular PP film was performed via chromic acid oxidation and then hydrofluoric acid treatment. Deep chemical modification is achieved as indicated by the energy-dispersive X-ray analyses on the cross-section of the modified cellular PP film. The results of the isothermal decay for piezoelectric d ₃₃-coefficient at 70°C indicate the improved thermal stability of piezoelectricity and the enhanced piezoelectric activity of the modified PP ferroelectrets. The former is attributed to the improvement of thermal stability of the charges trapped in the internal void surface layers as indicated by the thermally stimulated discharge measurements, while the latter results not only from the improved thermal stability of the charges but also from the reduction in Young’s modulus of the PP ferroelectrets due to the chemical modification as revealed by the dielectric resonance analyses.     

Structural and ionic conductivity studies on proton conducting polymer electrolyte based on polyvinyl alcohol

An attempt has been made to prepare a new proton conducting polymer electrolyte based on polyvinyl alcohol (PVA) doped with NH₄NO₃ by solution casting technique. The complex formation between polymer and dissociated salt has been confirmed by X-ray diffraction analysis. The ionic conductivity of the prepared polymer electrolyte has been found by ac impedance spectroscopic analysis. The highest ionic conductivity has been found to be 7.5 × 10⁻³ Scm⁻¹ at ambient temperature for 20 mol% NH₄NO₃-doped PVA with low activation energy (~0.19 eV). The temperature-dependent conductivity of the polymer electrolyte follows an Arrhenius relationship, which shows hopping of ions in the polymer matrix.