Thermally stimulated discharge conductivity in polymer composite thin films

This paper describes the results of thermally stimulated discharge conductivity study of activated charcoal-polyvinyl chloride (PVC) thin film thermoelectrets. TSDC has been carried out in the temperature range 308–400°K and at four different polarizing fields. Results are discussed on the basis of mobility of activated charcoal and polyvinyl chloride chains.     

Electret effect in Pb<Subscript>5</Subscript>Ge<Subscript>3</Subscript>O<Subscript>11</Subscript> crystals

The short-circuit thermally stimulated depolarization current (TSDC) through lead germanate single crystals has been measured as a function of temperature (100–800 K) and time. The results indicate that poling of the crystals at elevated temperatures (t ≥ 150°C) produces an electret state related to the spacecharge mechanism of polarization. Relatively mild poling conditions (E = 0.75 kV/cm, t = 150°C) produce a well-defined, long-lived electret with an abnormally large electret charge (1400 μC/cm²). The electret discharge leads to heating of the crystal, in the form of a peak in the range 520–570 K, whose height exceeds that of the pyroelectric peak near T _C by two to three orders of magnitude. From the TSDC data, we evaluated the stored electret charge, its density, and the activation energy of traps for electret charges, and made preliminary conclusions as to the nature of the traps. We demonstrate that neglect of the electret discharge current (which depends on a number of factors) when determining the pyroelectric coefficient p ^σ above 280 K leads to a significant scatter in data.     

Structural, microstructural and dielectric studies of tin-doped barium niobate perovskite

Monophasic oxides of the type Ba(Nb_1-x Sn _x ) O₃ (0 ≤ x ≤ 1) have been synthesized by solid-state reaction method. All these compounds are found to have tetragonal structure except x = 1. The cell parameters and their variation with composition x have been determined. The X-ray density is found to increase gradually with increase of dopant concentration. Tolerance factor and volume of unit cell was found to be almost constant for all the compositions. Scanning electron microscopy showed the presence of grains of approximately 1 μm in size. Dielectric measurements in the frequency range 100 Hz to 1 MHz and in the temperature range from − 100°C to 500°C has been carried out to determine the dielectric parameters. A strong frequency dependence of both dielectric constant (ɛ′) and dielectric loss (D) is observed in the frequency range 100 Hz to 100 kHz. At low frequency, the piling up of mobile charge carriers at the grain boundary produces interfacial polarization giving rise to high dielectric constant. Dielectric loss showed a typical behaviour in the temperature and frequency range studied.     

Dielectric properties of a ceramic oxide: Li(Ni<Subscript>7/10</Subscript>Fe<Subscript>3/10</Subscript>)VO<Subscript>4</Subscript>

The Li(Ni_7/10Fe_3/10)VO₄ compound has been synthesized by solution-based chemical route. Its dielectric response is investigated using complex impedance spectroscopy technique. Frequency dependence of dielectric constant (ε_r) at different temperatures shows low-frequency dispersion due to polarized structure of the material and mobile charge carriers. Temperature dependence of ε_r at different frequencies exhibits the dielectric anomalies in ε_r at different temperatures. Dielectric relaxation process in the material is signified by the variation of tangent loss with frequency at different temperatures. The variation of relaxation time with temperature obeys the Vogel–Fulcher law.     

Effect of paramagnetic manganese ions doping on frequency and high temperature dependence dielectric response of layered Na<Subscript>1·9</Subscript>Li<Subscript>0·1</Subscript>Ti<Subscript>3</Subscript>O<Subscript>7</Subscript> ceramics

The manganese doped layered ceramic samples (Na_1·9Li_0·1)Ti₃O₇ : XMn(0·01 ≤ X ≤ 0·1) have been prepared using high temperature solid state reaction. The room temperature electron paramagnetic resonance (EPR) investigations exhibit that at lower percentage of doping the substitution of manganese ions occur as Mn³⁺ at Ti⁴⁺ sites, whereas for higher percentage of doping Mn²⁺ ions occupy the two different interlayer sodium/lithium sites. In both cases, the charge compensation mechanism should operate to maintain the overall charge neutrality of the lattice. The manganese doped derivatives of layered Na_1·9Li_0·1Ti₃O₇ (SLT) ceramics have been investigated through frequency dependence dielectric spectroscopy in this work. The results indicate that the dielectric losses in these ceramics are the collective contribution of electric conduction, dipole orientation and space charge polarization. Smeared peaks in temperature dependence of permittivity plots suggest diffuse nature of high temperature ferroelectric phase transition. The light manganese doping in SLT enhances the dielectric constant. However, manganese doping decreases dielectric loss due to inhibition of domain wall motion, enhances electron-hopping conduction, and impedes the interlayer ionic conduction as well. Manganese doping also gives rise to contraction of interlayer space.     

Dielectric behaviour of erbium substituted Mn-Zn ferrites

Dielectric properties such as dielectric constant (ε′) and dielectric loss tangent (tan□δ) of mixed Mn-Zn-Er ferrites having the compositional formula Mn_0.58Zn_0.37Fe_2.05−xEr_x0₄ (where itx = 0.2, 0.4, 0.6, 0.8 and 1.0) were measured at room temperature in the frequency range 1–13 MHz using a HP 4192A impedance analyser. Plots of dielectric constant (ε′) vs frequency show a normal dielectric behaviour of spinel ferrites. The frequency dependence of dielectric loss tangent (tan δ) was found to be abnormal, giving a peak at certain frequency for all mixed Mn-Zn-Er ferrites. A qualitative explanation is given for the composition and frequency dependence of the dielectric constant and dielectric loss tangent. Plots of dielectric constant vs temperature have shown a transition near the Curie temperature for all the samples of Mn-Zn-Er ferrites. However, Mn_0.58Zn_0.37Er_1.0Fe_1.05O₄ does not show a transition. On the basis of these results an explanation for the dielectric mechanism in Mn-Zn-Er ferrites is suggested.     

Electrical properties of R<Subscript>2</Subscript>O–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–SiO<Subscript>2</Subscript> glass–ceramics for anodic bonding

Temperature and frequency dependence on electrical properties (dielectric constant, dielectric loss and conductivity) of Li₂O–Na₂O–K₂O–Al₂O₃–SiO₂(R₂O–Al₂O₃–SiO₂) system glass–ceramics used as anodic bonding materials were discussed. The results showed that the main crystal phase of glass–ceramics was lithium metasilicate (Li₂SiO₃). Compared with the parent glass, both the dielectric constant and dielectric loss of glass–ceramics decreased, the dielectric constant and dielectric loss increased gradually with the increasing of the test temperature from room temperature to 400 °C, Testing frequency (30–300 MHz) had very little influence on the dielectric properties of samples. The electrical conductivity of glass–ceramics showed a trend of first decrease and then increase with the increasing of temperature. The glass–ceramics which has a lower dielectric constant, dielectric loss and better stability under high frequency was obtained after an appropriate heat treatment; it could be used as anodic bonding materials under very high frequency.     

Open- and short-circuit thermally stimulated currents in ethyl cellulose (EC): polymethyl methacrylate (PMMA) blend

Mechanisms of charge generation and its persistence in one and both-side vacuum-aluminized ethyl cellulose (EC):polymethyl methacrylate (PMMA) blend thermoelectrets, prepared under different fields (10, 25, 50 and 100 kV/cm) and temperatures (40, 60, 80 and 100°C), have been analysed using short- and open-circuit thermally stimulated depolarization current (TSDC) technique. The TSDCs were recorded by reheating the samples at a linear heating rate of 4°C/min. The TSDC thermograms of polyblends containing EC:PMMA in different weight ratio are, in general, characterized with two peaks in lower and higher temperature regions. However, the polarity of the peaks was found to be just opposite in short- and open-circuit TSDC measurements. Moreover, results on 97:3, 93:7 and 90:10 EC:PMMA polyblends indicated that the current increases with concentration of PMMA. The results indicate the existence of heterocharge due to dipole orientation and ionic charge drift together with the injection of charge carriers from electrodes with their subsequent localization in surface and bulk traps. Further, the chances of charge trapping in polyblends, at the interfaces are greater than in the individual polymers.     

Synthesis and dielectric properties of MXTi<Subscript>7</Subscript>O<Subscript>16</Subscript> (M = Ba and Sr; X = Mg and Zn) hollandite ceramics

MXTi₇O₁₆ (M = Ba and Sr; X = Mg and Zn) ceramics have been synthesized by the conventional solid state ceramic route. The dielectric properties such as dielectric constant (ε_r), loss tangent (tan δ) and temperature variation of dielectric constant (τ_εr) of the sintered ceramic compacts are studied using an impedance analyser up to 13 MHz region. The strontium compounds have relatively high dielectric constant and low loss tangent compared to the barium analogue. The phase purity of these materials has been examined using X-ray diffraction studies and microstructure using SEM method.     

Electrical properties and scaling behaviour of Sm<Superscript>3 + </Superscript> doped CaF<Subscript>2</Subscript>-bismuth borate glasses

The electrical properties for 20Bi₂O₃–60B₂O₃ (20−x)–CaF₂–xSm₂O₃ glasses (0 ≤ x ≤ 2) were measured in the temperature range 297 K up to 629 K and in the frequency range 0·1–100 kHz. The d.c. and a.c. conductivity values and the dielectric loss (tan δ) values were found to increase with increasing Sm₂O₃ content, whereas the activation energy of conductivities and the dielectric constant decreased. These results were attributed to the introduction of the rare earth ions; promote the formation of a high number of non-bridging oxygen atoms, which facilitate the mobility of charge carriers. The frequency dependence of the a.c. conductivity follows the power law σ _ac(ω) = Aω ^s . The frequency exponent (s) values (0·64 < s < 0·8) decrease with increasing temperature. This suggested that the a.c. conduction mechanism follows the correlated barrier hopping model (CBH). The dielectric constant (ε ^′) and dielectric loss (tan δ values) were found to increase with increasing temperature and increasing Sm₂O₃ concentration in the glass. The a.c. conductivities as a function of frequency at different temperatures of a given glass superimposed onto a master curve (Roling scaling model). Furthermore, we have performed to scale the data as a function of composition. Two master curves were obtained, which suggested that there are differences in dominant charge carriers between glasses having Sm₂O₃ concentration ≥1 and glass of Sm₂O₃ concentration <1.     

Strain-induced artificial multiferroicity in Pb(Zr<Subscript>0.53</Subscript>Ti<Subscript>0.47</Subscript>)O<Subscript>3</Subscript>/Pb(Fe<Subscript>0.66</Subscript>W<Subscript>0.33</Subscript>)O<Subscript>3</Subscript> layered nanostructure at ambient temperature

Layered nanostructures (LNs) of the commercial ferroelectric Pb(Zr_0.53Ti_0.47)O₃ (PZT) and the natural ferroic relaxor Pb(Fe_0.66W_0.33)O₃ (PFW) were fabricated with a periodicity of PZT/PFW/PZT (~5/1/5 nm, thickness ~250 nm) on MgO substrates by pulsed laser deposition. The dielectric behavior of these LNs were investigated over a wide range of temperatures and frequencies, observing Debye-type relaxation with marked deviation at elevated temperatures (>400 K). High dielectric constant and very low dielectric loss were observed below 100 kHz and 400 K, whereas the dielectric constant decreases and loss increases with increase in frequency, similar to relaxor ferroelectrics. Asymmetric ferroelectric hysteresis loops across UP and DOWN electric field were observed with high remanent polarization (P_r) of about 33 μC/cm². High imprint (~5–7 V across 250 nm thin films) were seen in ferroelectric hysteresis that may be due to charge accumulation at the interface of layers or significant amount of strain (~3.21) across the layers. Room temperature ferromagnetic hysteresis was observed with remanent magnetization 5.32 emu/cc and a coercive field of ~550 Oe. Temperature and field dependent leakage current densities showed very low leakage ~10⁻⁷–10⁻⁵ A/cm² over 500 kV/cm. We observed imprint in hysteresis that may be due to charge accumulation at the interface of layers or active role of polar nano regions (PNRs) situated in the PFW regions.     

Dielectric relaxation in Se<Subscript>80−<Emphasis Type="Italic">x</Emphasis></Subscript>Te<Subscript>20</Subscript>Sn<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> chalcogenide glasses

This study reports the temperature and frequency dependence of dielectric constant (ε′) and dielectric loss (ε′′) in glassy Se_80−x Te₂₀Sn _x (x = 0, 2, 4, 6) alloys. The measurements have been made in the frequency range (1–500 KHz) and in the temperature range 305–335 K. The results indicate that the dielectric dispersion exists in the present glassy systems in the above frequency and temperature range. The composition dependence of the dielectric constant, dielectric loss and activation energy thermally activated crystallization is also discussed.     

Enhanced microwave dielectric properties of Ba<Subscript>0.40</Subscript>Sr<Subscript>0.60</Subscript>TiO<Subscript>3</Subscript>–Zr<Subscript>0.80</Subscript>Sn<Subscript>0.20</Subscript>TiO<Subscript>4</Subscript> composite ceramics

The (1−x) Ba_0.40Sr_0.60TiO₃ (BST)−xZr_0.80Sn_0.20TiO₄ (ZST) composite ceramics with x = 10, 20, 30, and 40 wt% were fabricated by conventional solid-state reaction method. With increasing of ZST content, the dielectric constant of composite ceramics was decreased and dielectric loss increases. The effect of ZnO addition to 70 wt% BST–30 wt% ZST composition on the microstructure and dielectric properties was investigated. The improvements in dielectric constant, dielectric loss, and microwave dielectric properties of composite ceramics can be achieved by ZnO addition. The sample with 98 wt% (70 wt% BST–30 wt% ZST)–2 wt%ZnO composition exhibits promising dielectric properties, with dielectric constant, loss tangent and tunability at 4 kV/mm, of 125, 0.0016 and 12%, at 10 kHz and room temperature. At ~2 GHz, it possesses a dielectric constant of 101 and a Q factor of 187, which makes it a good candidate for tunable microwave device applications.     

The effect of sintering temperature on magnetic and dielectric properties of Ho<Subscript>3</Subscript>Fe<Subscript>5</Subscript>O<Subscript>12</Subscript> ceramics

Ho₃Fe₅O₁₂ ceramics were fabricated by the solid-state reaction method. The results revealed an increase of the grain size, dielectric constant, and dielectric loss, while a decrease of the remnant magnetization and coercive field with increasing sintering temperature. A dielectric relaxation behavior was observed, which might be associated with the charge carrier hopping between Fe²⁺ and Fe³⁺. A cole–cole fitting to loss peaks revealed a dependence of the activation energy and the broaden factor on the relative density of the samples. Furthermore, at appropriate frequencies, the 1250 °C-sintered samples showed high dielectric constant, low dispassion, and good temperature stability around room temperature.     

Effect of layer charge on chemical and physical properties of synthetic K-fluorine micas

The fluorine micas (K-fluorine micas; K_XMg_3-XLi_XSi₄O₁₀F₂) having variable layer charges (x = 0.4–1.0) were synthesized. The lattice constant c decreased with a decrease in the layer charge while the lattice constants a and b increased. As the layer charge decreased, K-fluorine micas were changed into Na-fluorine micas more rapidly by NaB(C₆H₅)₄ treatment and were easier to cleave and change into the amorphous phase by grinding. The mica ceramics with lower layer charges showed lower electrical resistance than those with higher layer charges in the low-temperature region but higher electrical resistance in the high-temperature region. The results of the electrical resistance can be explained by the concentrations of the lattice vacancy and K⁺ ion in the interlayer. The dielectric loss tangent was influenced by the layer charge while the dielectric constant was almost unchanged. The chemical and physical properties of such micas are strongly dependent on the magnitude of the layer charge because the layer charge determines the interlayer bonding strength and the stability of mica structure.     

Dielectric properties of electron irradiated PbZrO<Subscript>3</Subscript> thin films

The present paper deals with the study of the effects of electron (8 MeV) irradiation on the dielectric and ferroelectric properties of PbZrO₃ thin films grown by sol-gel technique. The films were (0.62 μm thick) subjected to electron irradiation using Microtron accelerator (delivered dose 80, 100, 120 kGy). The films were well crystallized prior to and after electron irradiation. However, local amorphization was observed after irradiation. There is an appreciable change in the dielectric constant after irradiation with different delivered doses. The dielectric loss showed significant frequency dispersion for both unirradiated and electron irradiated films. T _c was found to shift towards higher temperature with increasing delivered dose. The effect of radiation induced increase of ɛ′(T) is related to an internal bias field, which is caused by radiation induced charges trapped at grain boundaries. The double butterfly loop is retained even after electron irradiation to the different delivered doses. The broader hysteresis loop seems to be related to radiation induced charges causing an enhanced space charge polarization. Radiation-induced oxygen vacancies do not change the general shape of the AFE hysteresis loop but they increase P _s of the hysteresis at the electric field forced AFE to FE phase transition. We attribute the changes in the dielectric properties to the structural defects such as oxygen vacancies and radiation induced charges. The shift in T _C, increase in dielectric constant, broader hysteresis loop, and increase in P _r can be related to radiation induced charges causing space charge polarization. Double butterfly and hysteresis loops were retained indicative of AFE nature of the films.     

BaTiO3 (BTO)–CaCu3Ti4O12 (CCTO) substrates for microwave devices and antennas

The solid state procedure was used to produce bulk ceramics of BTO (BaTiO₃), CCTO (CaCu₃Ti₄O₁₂) and BTO_0.5–CCTO_0.5 that were studied in the medium-frequency (MF) range (100 Hz–1 MHz) and in the microwave range of frequencies. The presence of BTO is decreasing the dielectric constant (ε_r) of the BTO–CCTO composite. The CCTO and BTO samples present a strong tendency to the increase of the loss with frequency. The BTO substrates are presenting higher values of the ε_r in the range of 1–4 GHz (around 140). For pure CCTO the dielectric constant is around 37.6. Similar behaviour observed at the MF range, that the higher dielectric constant is also associated to the higher loss is also present in the microwave region. The study of a planar microstrip antenna, that uses the BTO _X –CCTO_(1−X) ceramic as a high ε_r substrate was done. Therefore, these measurements confirm the potential use of such materials for small high dielectric planar antennas (HDA). These materials are also very promising for capacitor applications and certainly for microelectronics, microwave devices (cell mobile phones for example), where the miniaturization of the devices is crucial.     

Preparation,characterization and dielectric behaviour of some yttrium doped strontium stannates

Samples of Sr_{(1− 3x/2)}YxSnO₃ are prepared by usual solid state reaction route. X- ray diffraction studies confirm the formation of single cubic perovskite single phase. The dielectric constant and dielectric loss at 1 kHz were measured in the temperature range from room temperature up to -150†C. The dielectric constant decreases and losses increase with increased yttrium content in the samples. The percentage porosity and unit cell parameters are also calculated for the samples.     

Perovskite-type oxides as susceptor materials in dielectric heating

Dielectric properties of La_1−x Ce _x MnO₃ perovskites are investigated in order to assess the heating behaviour in the wider context of the use of perovskite coatings in microwave assisted soot filter regeneration. Dielectric permittivities in the radio and microwave region for these perovskites were determined at room temperature. The dielectric constant and dielectric loss are related to ionic conduction at low frequencies, while at microwave frequencies storage and loss mainly proceed through reorientation of molecular dipoles. The dielectric constant rises for a higher degree of La substitution by Ce, which is explained by an increase of the number of cation/oxygen vacancies. Concurrently the mean perovskite crystallite size decreases, which is possibly related to defect formation. The dielectric constant declines for x ≥ 0.3, along with the formation of a separate, low dielectric permittivity CeO₂ phase. The La–Ce–Mn perovskites are further shown to exhibit a high thermal stability during repeated heating/cooling cycles.     

Dielectric and thermal studies on gel grown strontium tartrate pentahydrate crystals

Results of dielectric and thermal studies on strontium tartrate pentahydrate crystals are described. The value of dielectric constant is shown to be independent of temperature till 360 K at all the frequencies (110–700 kHz) of the applied a.c. field. It increases abruptly achieving a peak value of 25.5 at 100 kHz; the peak value being strongly dependent on frequency. In the temperature range, 87 < T < 117°C, the value of ɛ′ falls suggesting a transition at around 100°C or so. The dielectric constant, ɛ′, of the material is shown to be frequency dependent but temperature independent in the pre- or post-T _c range 87 < T < 117°C, suggesting that the contribution towards polarization may be due to ionic or space charge polarization which gets eliminated at higher frequencies. The ferroelectric transition is supported by the results of thermoanalytical studies. It is explained that crystallographic change due to polymorphic phase transition may be occurring in the material, besides the change due to loss of water molecules, which leads to the dielectric anomaly at around 100°C. Coats-Redfern approximation method is applied for obtaining non-isothermal kinetic parameters leading to calculation of activation energies corresponding to three decomposition stages of material in the temperature ranging from 379–1113 K.