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.     

Evaluation of a.c. conductivity behaviour of graphite filled polysulphide modified epoxy composites

Composites of epoxy resin having different amounts of graphite particles have been prepared by solution casting method. Temperature dependence of dielectric constant, tan δ and a.c. conductivity was measured in the frequency range, 1–20 kHz, temperature range, 40–180°C for 0.99, 1.96 and 2.91 wt% graphite filled and unfilled epoxy composites. It was observed that the dielectric constant, tanδ and a.c. conductivity increase with increasing temperature. Near the transition temperature the materials show anomalous behaviour for the observed properties. Peaks of dielectric constant, tan δ and a.c. conductivity were observed to shift towards lower temperature with increasing frequency. Clear relaxation (tan δ) peaks around 169°C were observed in epoxy resin, which shifted to lower temperature side on increasing the frequency. Addition of 2.91 wt% graphite shifted the tan δ peaks towards higher temperature side by creating hindrances to the rotation of polymer dipoles. Addition of 2–91 wt% graphite leads to an increased relaxation time τ of dipoles in polysulphide epoxy from 1.44 × 10⁻⁵− 3.92 × 10⁻⁵ (s) at 90°C by creating the hindrance to the rotation of dipoles.     

Dielectric behaviour of strontium tartrate single crystals

Strontium tartrate trihydrate (STT) crystals have been grown in silica hydrogel. Various polarization mechanisms such as atomic polarization of lattice, orientational polarization of dipoles and space charge polarization in the grown crystals have been understood using results of the measurements of dielectric constant (έ′) and dielectric loss (tan δ) as functions of frequency and temperature. Ion core type polarization is seen in the temperature range 75–180°C, and above 180°C, there is interfacial polarization for relatively lower frequency range. One observes dielectric dispersion at lower frequency presumably due to domain wall relaxation.     

Dielectric and complex impedance studies of BaTi<Subscript>0·85</Subscript>W<Subscript>0·15</Subscript>O<Subscript>3+<Emphasis Type="BoldItalic">δ</Emphasis></Subscript> ferroelectric ceramics

In the present work, tungsten substituted barium titanate have been synthesized and studied. The structural analysis indicates that the specimen is a single phase material with tetragonal crystal structure. The observed polarization–electric field hysteresis loop confirms the ferroelectric nature of the prepared compound. Variation of dielectric constant with temperature at different frequencies shows that the compound has a dielectric anomaly at 75 °C and exhibits diffuse type phase transition. Variation of dielectric loss with temperature at different frequencies shows a decrease in loss with increasing frequency. The Nyquist plots (Cole–Cole plots) have been measured at temperatures 325 °C, 345 °C and 365 °C. The plot at 365 °C shows a grain boundary effect. Relaxation time has been found to decrease with the rise in temperature and obey the Arrhenius relationship. The variations of d.c. conductivity as a function of temperature have also been studied.     

Dielectric properties of Na<Subscript>1-<Emphasis Type="Italic">x</Emphasis></Subscript>K<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>NbO<Subscript>3</Subscript> in orthorhombic phase

Pellets of ceramic Na_1−xK_xNbO₃ (x = 0, 0.2 and 0.5), were prepared by conventional solid-state reaction method. Prepared samples were characterized using XRD and SEM. The frequency and temperature variation of dielectric constant, loss tangent and dielectric conductivity of prepared samples were measured in the frequency range from 10 KHz-1 MHz, and in the temperature range from 50–250°C for x = 0.2 and 0.5, and between 50 and 480°C for x = 0 compositions. It was observed that the dielectric constant and loss tangent decrease, and conductivity increases with increasing frequency. Near the transition temperature the material shows anomalous behaviour for the observed properties, and the peaks of dielectric constant and loss tangent were observed shifting towards lower temperature with increasing frequency.     

Dielectric characterization of gadolinium tartrate trihydrate crystals

Single crystals of gadolinium tartrate trihydrate have been grown by gel diffusion technique. Single crystal X-ray diffraction analysis shows that the crystals belong to the tetragonal system with non-centrosymmetric space group. The dielectric constant, dielectric loss and ac conductivity have been measured as a function of frequency in the range 1 kHz–5 MHz and temperature range 20–300 °C. The dielectric constant increases with temperature, attains a peak around 240 °C and then decreases as the temperature exceeds 240 °C. The dielectric anomaly at 240 °C is suggested to be due to phase transition brought about in the material, which is further supported by the thermal studies. The variation of ac conductivity with temperature has been measured and the material is suggested to show protonic conductivity.     

Electrical properties of ion irradiated polypropylene films

The effect of high-energy (50 MeV) Li³⁺ ion beam irradiation on polypropylene (PP) film has been studied in the fluence range 2.4 × 10¹²−l.5 × 10¹⁴ ions/cm². The a.c. electrical properties of PP films were measured in the frequency range from 0.05– 100 kHz, and at temperature range between 30 and 140°C. This study indicates two peaks at 60°C and 120°C with comparatively high magnitudes. There is an exponential increase in conductivity with log of frequency and the effect is significant at higher fluences. The loss factor (tan δ) vs frequency plot suggests that PP film based capacitors may be useful below 10 kHz. The capacitance is constant over a wide temperature range up to 130°C. FTIR spectra of the PP films before and after irradiation indicate that intensity of C-H stretching vibration at 2900 cm⁻¹ is modified. The presence of many new peaks with the increase of fluence suggests the formation of alkanes and alkynes which might be responsible for the observed changes in the dielectric and electrical properties of PP films.     

Structure and dielectric properties of potassium niobate nano glass–ceramics

Glasses in the composition of 25K₂O-25Nb₂O₅-50SiO₂ (mol %) have been prepared by melt quenching technique and isothermally heat-treated at 800 °C for different duration (0–200 h). The formed nanocrystalline KNbO₃ phase, crystallite size and morphology are examined by X-ray diffraction, Fourier transform infrared reflection spectroscopy, field emission scanning and transmission electron microscopes. The frequency and temperature dependent dielectric constant and loss tangent are measured in the frequency and temperature ranges 0.1–1000 kHz and 200–500 °C respectively. The dielectric constant and loss tangent are found to decrease with increasing frequency and increase with increasing temperature. The dielectric constant and loss tangent versus temperature curve at different frequency revealed the phase transition of KNbO₃ from paraelectric cubic to ferroelectric tetragonal around 425 and 397 °C (Curie temperature) for nano glass–ceramics obtained after 1 and 200 h heat-treatment respectively.     

Thermally stimulated current and electrical conduction in metal (1)-ethyl cellulose-metal (1)/(2) systems

Depolarization current characteristics of solution grown pure ethyl cellulose (EC) films of about 20μm thickness have been studied as a function of electrode materials at constant poling field (5 × 10⁴ V/cm) and poling temperature 40°C. Thermally stimulated current (TSC) thermograms of EC consists of two well resolved peaks (located at 60°C and 140°C) for Al-Al system, which are attributed to the deorientation of strongly attached ethoxy groups of glycosidal units and diffusion of space charges either at electrodes or due to their thermal release at higher temperatures from the defect levels. For dissimilar electrode combinations (Al-Ag/Cu/Au/Sn/Pb), an indication of peak of lower magnitude at around (50–70°C) alongwith a higher temperature peak (140–155°C), have been observed. TSC parameters are found to change with the choice of electrode material. The dependence of dark current at 40°C in metal-ethyl cellulose-metal systems on applied voltage in the range (2·0–5·0) × 10⁴V/cm has also been studied. The results of current-voltage measurement on EC have been interpreted to show that the Schottky-Richardson mechanism is the controlling transport mechanism. Zero field current density extrapolated fromI-E ^1/2 plots are found to vary with metal work function.     

Characterization and analysis of CaO–SiO<Subscript>2</Subscript>–B<Subscript>2</Subscript>O<Subscript>3</Subscript> ternary system ceramics

The dielectric, thermal and mechanical properties of CaO–SiO₂–B₂O₃ ternary system ceramics by solid-phase method have been carried out and quantitive analysis been examined by X-ray diffraction (XRD) patterns. The results showed that the major crystalline phase of CaO–SiO₂–B₂O₃ ternary system ceramics was wollastonite (about 90 wt%) which existed at the temperature ranging from 950 to 1,100 °C. It is also observed that wollastonite could be transformed to pseudowollastonite at 1,200 °C. In addition, with increase in calcination temperature, the amount of wollastonite increases. When the sintering temperature is at 1,100 °C, the amount of wollastonite has a maximum value of 92.7 wt%. Accordingly, CaO–SiO₂–B₂O₃ ternary system ceramics achieved excellent properties at 1,100 °C, such as dielectric constant of 8.38, dielectric loss of 1.51 × 10⁻³ at 1 MHz, linear thermal-expansion coefficient (300 K) of 6.68 × 10⁻⁶/K, bending strength of 121.75 Mpa. Analysis of the mechanical and dielectric properties showed that the measured bending strength, dielectric constant and loss of CaO–SiO₂–B₂O₃ ternary system ceramics can be substantially modified and improved by controlling the sintering temperature, in particular due to the amount of wollastonite crystalline phase and size of grains.     

Effect of replacement of MgO by CaO on sintering,crystallization and properties of MgO–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–SiO<Subscript>2</Subscript> system glass-ceramics

The effects of replacement of MgO by CaO on the sintering and crystallization behavior of MgO–Al₂O₃–SiO₂ system glass-ceramics were investigated. The results show that with increasing CaO content, the glass transition temperature firstly increased and then decreased, the melting temperature was lowered and the crystallization temperature of the glass-ceramics shifted clearly towards higher temperatures. With the replacement of MgO by less than 3 wt.% CaO, the predominant crystalline phase in the glass-ceramics fired at 900 °C was found to be α-cordierite and the secondary crystalline phase to be μ-cordierite. When the replacement was increased to 10 wt.%, the predominant crystalline phase was found to be anorthite and the secondary phase to be α-cordierite. Both thermal expansion coefficient (TCE) and dielectric constant of samples increases with the replacement of MgO by CaO. The dielectric loss of sample with 5 wt.% CaO fired at 900 °C has the lowest value of 0.08%. Only the sample containing 5 wt.% and10 wt.% CaO (abbreviated as sample C5 and C10) can be fully sintered before 900 °C. Therefore, a dense and low dielectric loss glass-ceramic with predominant crystal phase of α-cordierite and some amount of anorthite was achieved by using fine glass powders (D₅₀ = 3 μm) fired at 875–900 °C. The as-sintered density approaches 98% theoretical density. The flexural strength of sample C5 firstly increases and then decreases with sintering temperature, which closely corresponds to its relative density. The TCE of sample C5 increases with increasing temperature. The dielectric property of sample C5 sintered at different temperatures depends on not only its relative density but also its crystalline phases. The dense and crystallized glass-ceramic C5 exhibits a low sintering temperature (≤900 °C), a fairly low dielectric constant (5.2–5.3), a low dielectric loss (≤10⁻³) at 1 MHz, a low TCE (4.0–4.25 × 10⁻⁶ K⁻¹), very close to that of Si (∼3.5 × 10⁻⁶ K⁻¹), and a higher flexural strength (≥134 MPa), suggesting that it would be a promising material in the electronic packaging field.     

Structure and dielectric properties of a new series of pyrochlores in the Ca–Sm–Ti–M–O (M = Nb and Ta) system

The present work investigates the dielectric properties of pyrochlore type oxides, Ca–Sm–Ti–M–O (M = Nb and Ta) in the low frequency region (100 Hz–1 MHz) over the temperature range 30–100 °C. The 1 MHz dielectric constants (K) of these oxides are in the range 23–108 and show low variation with frequency (1 kHz–1 MHz). The temperature coefficient of dielectric constant (TCK) over the temperature range varies from positive to negative values in the range 48 to −107 ppm/°C. Rietveld analysis of the X-ray diffraction data establishes a cubic pyrochlore-type phase in the space group Fd3 m (no. 227).The grain morphology observation by scanning electron microscope shows well sintered grains.     

Preparation of forsterite-based glass ceramics for LTCC from potassium feldspar

A forsterite-based glass ceramic material has been developed from potassium feldspar for low temperature co-fired ceramics (LTCC). The crystalline phases and microstructure of forsterite-based glass ceramics were investigated using X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). The results show only forsterite was formed in temperature range 900–1,050 °C, and sapphirine was formed in temperature range 1,080–1,100 °C. The glass compact could be well densified at 950 °C, and full densification samples were obtained in temperature range 1,000–1,050 °C. The physical properties including dielectric properties, bending strength and thermal expansion of the specimens were also evaluated. The dielectric constants are in the range 7.00–8.25 and dielectric loss is below 0.01 in the frequency range 1–10 MHz. The specimens obtained in temperature range 950–1,100 °C are of high bending strength (69–106 MPa). The linear coefficient of thermal expansion of the specimen sintered at 1,080 °C is 9.76 × 10^?6 K^?1. All of these qualify the forsterite-based glass ceramic for further investigation as a candidate suitable for applications in LTCC field.     

Poly(acrylic acid) + zinc diacetate composites: High temperature service and electric conductivity

Poly(acrylic acid) + zinc diacetate hybrid composites have been prepared by precipitation from aqueous solutions and drying. The lowest glass transition temperature T_g determined by differential scanning calorimetry (DSC) is 392°C, providing a service temperature range unusually large for polymer-based materials (PBMs). Thermogravimetric analysis (TGA) shows that thermal decomposition begins some 10–20 K above each T_g. The alternating current impedance was determined in the nitrogen atmosphere from 370°C to 530°C. Dynamic dielectric measurements were performed between 20°C and 350°C, also under nitrogen. In contrast to typical PBMs, there is evidence of ionic conduction in some of the composites. The dynamic dielectric properties depend on the composition. The materials obtained are usable in medical applications and as high durability low friction coatings. Received: 19 February 1999 / Reviewed and accepted: 13 March 1999     

Dielectric,ferroelectric and optical behaviour of terbium hydrogen tartrate trihydrate crystals

Gel diffusion technique, using agar–agar as gel medium, has been employed to obtain single crystals of terbium hydrogen tartrate trihydrate. The grown crystals are characterised by X-ray diffraction, scanning electron microscopy, CHN technique, thermogravimetric methods and UV–Vis spectroscopy. Dielectric, ferroelectric and optical studies on this metal–organic compound have been carried out. The dielectric constant has been measured as a function of temperature and frequency in the ranges of 20–250 °C and 20 Hz–3 MHz, respectively. The study of dielectric behaviour as a function of temperature reveals two dielectric anomalies at 95 and 198 °C. The dielectric anomaly at 95 °C is suggested to be due to ferroelectric phase transition brought about in the material. The study of polarisation versus electric field shows a hysteresis loop which thereby confirms the ferroelectric nature of terbium hydrogen tartrate trihydrate crystals. The dielectric anomaly at 198 °C is suggested to be due to loss of water molecules in the compound. The results of thermal study show that the material is thermally stable up to temperature of about 200 °C. Optical studies show that the terbium hydrogen tartrate trihydrate crystal has good transparency in the entire visible and infra red range of the spectrum.     

Variation of electrical properties in sepiolite during dehydration

The dielectric constant (K), loss (tanδ) andac conductivity of a sepiolite sample have been measured as a function of frequency in the range 10²-10⁷ Hz and in the temperature region 30–400°C. Thedc conductivities of hot pressed pellets were measured in the temperature range 30–550°C.K and tanδ of these samples decrease with increasing frequency. Results of these measurements have been correlated with the structural transformation accompanying dehydration, making use ofdta, ir and x-ray data. The moderately large value of activation energy (∼ 2·2 eV) in the intrinsic range suggests that the conduction process is most probably associated with ions.     

Low-temperature-sintering and characterization of glass-ceramic composites

To meet the demands of high power and high-speed propagation of the signal for very large scale integration, a series of glass/ceramic composites were prepared using electronic ceramics process from borosilicate glass with Sr-celsian, which contains 30, 40, 50, 60, 70 wt% ceramic. The phase and microstructural evolution of the composites were characterized by XRD and SEM. The properties of the composites were also measured. Results show that the thermal expansion coefficient, dielectric constant and hardness of the composites increase with an increase content of Sr-celsian. However, the dielectric loss decreases with increasing Sr-celsian content. For the composites with ≧ 60 wt% Sr-celsian fired at 850–900°C, formation of α-quartz and cristobalite in the composites during the sintering process has bad effect on thermal expansion, but has little effect on the values of dielectric properties of the composites. The obtained composites exhibit low dielectric constant (5.2–5.8), low dielectric loss (⩽ 0.25%), low thermal expansion coefficient (4.4–6.2 × 10⁻⁶°C⁻¹) and low-temperature sintering behavior (⩽900 °C), which suit for electronic packaging field.     

Effect of temperature and frequency on the dielectric properties of cellulose nanofibers from cotton

The present work has been carried out to evaluate the dielectric properties and ac-electrical conductivity of cellulose nanofibers. The cellulose nanofibers (CNF) described in this work are the ones extracted from cotton via a simple acid hydrolysis method and are characterized with X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), and UV–Visible diffuse reflectance spectroscopy. The optical band gap of CNF found out using the Kubelka–Munk plot is 3.30 eV. The dielectric constant, dielectric loss, and ac-electrical conductivity of the prepared CNF have been investigated in the temperature range from 30 °C to 300 °C and in the frequency range from 50 Hz to 5 MHz. The synthesized system exhibits a higher dielectric constant value for all temperatures in the low-frequency (0.1 kHz) region and a frequency-independent behavior above 10 kHz. In the high-frequency region, the dielectric constant is independent of temperature. Also, the study shows that the conductivity increases with increasing frequency and temperature. The maximum values of ac-conductivity at room temperature (30 °C) and high temperature (300 °C) are found to be 4.58?×?10^–5 S/cm and 2.26?×?10^–4 S/cm, respectively. In brief, the studies point to the application potential of CNF for future flexible electronics.

     

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.     

Effect of ZnO addition on properties of cordierite-based glass-ceramics

The influences of addition of ZnO on sintering, crystallization behavior and properties of cordierite-based glass-ceramics were investigated. Results show that with increasing ZnO content, the batch melting temperature, glass transition temperature and crystallization temperature all decrease. Addition of ZnO can greatly improve the sinterability of the glass powders and alter the type of the crystalline phases. Addition of 1.5 wt% ZnO seems to be reasonable. Thermal expansion coefficients (TCEs) of samples increase with increasing ZnO contents. The density was found to be an important factor affecting the dielectric loss of the samples. Dielectric constant and TCEs of the sintered bulk samples were found to depend on their relative densities and crystalline phases. The samples doped with 1.5–3.0 wt% ZnO sintered at 950 °C has a low dielectric constant (5.0–5.2), a low dielectric loss (≤0.0018) and a low thermal expansion coefficient (3.6–4.8 × 10⁻⁶ K⁻¹), which are promising electronic packaging materials.