Evaluation of La<Subscript>2</Subscript>CoTi<Subscript>0.7</Subscript>Mg<Subscript>0.3</Subscript>O<Subscript>6</Subscript> as an electrode material for a symmetrical SOFC

La₂CoTi_0.7Mg_0.3O₆ (LCTM) material has been prepared at 1473 K for 24 h in air. X-ray powder diffraction study has revealed that it contains two orthorhombic perovskite phases (in a ratio ~1:4) with close unit cell parameters. Annealing of LCTM in reducing (Ar/H₂, 8%) atmosphere at 1173 K for 12 h has resulted in the preparation of a single-phase material containing the GdFeO₃-type perovskite phase with the unit cell parameters of a?=?5.5631(3) Å, b?=?5.5462(3) Å, c?=?7.8522(5) Å. LCTM material exhibits a reversible transformation of a mixture of two perovskite phases with close cation content in air and a single perovskite phase in a reducing atmosphere. Both as-prepared and reduced LCTM samples have been studied by thermogravimetric analysis and dilatometry in air and Ar/H₂ (8%). No chemical interaction between the as-prepared LCTM and standard electrolyte materials for SOFC like GDC and YSZ has been observed up to 1273 K. High-temperature electrical conductivity of the as-prepared LCTM at variable oxygen partial pressure (10^?4-0.21 atm) showed weak dependence over pO₂ with E_a?=?0.48?±?0.01 eV. AC impedance study of the symmetrical cells LCTM/GDC/LCTM has revealed ASR value at 1173 K of ~8.1?±?0.1 Ω?cm² in air and 0.24?±?0.05 Ω?cm² in a reducing atmosphere. These results allow to consider LCTM as a promising electrode material for a symmetrical SOFC.     

Coke-tolerant La<Subscript>2</Subscript>Sn<Subscript>2</Subscript>O<Subscript>7</Subscript>-Ni-Gd<Subscript>0.1</Subscript>Ce<Subscript>0.9</Subscript>O<Subscript>1.95</Subscript> composite anode for direct methane-fueled solid oxide fuel cells

Direct CH₄-fueled solid oxide fuel cells (SOFCs) have been studied for a few decades, but carbon depositions on the Ni-based anodes are still remained as a major problem. In order to enhance coke tolerances and durability of SOFCs, La₂Sn₂O₇ nano-powders are prepared by co-precipitation. The SOFCs with the different amounts of the La₂Sn₂O₇ nano-powders in the Ni-GDC anodes are tested under dry CH₄, and the 0.3 wt.% La₂Sn₂O₇-Ni-GDC (0.3LNG) anodes show the highest cell performances of all anodes. The maximum power density of the cell is approximately 0.55 W cm^?2 at 650 °C. The durability of the 0.3LNG cell is significantly enhanced without any carbon formations, showing approximately 0.69 V over 600 h at 0.3 A cm^?2, whereas the conventional Ni-GDC cell is stopped only after 90 h. It suggests that the 0.3LNG is a promising anode material to enhance coke-tolerances and durability of direct-methane fuel cells.     

Formation of a KNbO<Subscript>3</Subscript> single crystal using solvothermally synthesized K<Subscript>2-m</Subscript>Nb<Subscript>2</Subscript>O<Subscript>6-m/2</Subscript> pyrochlore phase

A K_2-mNb₂O_6-m/2 single crystal with a pyrochlore phase formed when the Nb₂O₅?+?x mol% KOH specimens with 0.6?≤?x?≤?1.2 were solvothermally heated at 230 °C for 24 h. They have an octahedral shape with a size of 100 μm, and the composition of this single crystal is close to K_1.3Nb₂O_5.65. The single-crystal KNbO₃ formed when the single-crystal K_2-mNb₂O_6-m/2 was annealed at a temperature between 600 °C and 800 °C with K₂CO₃ powders. When annealing was conducted at 600 °C (or with a small amount of K₂CO₃), the KNbO₃ single crystal has a rhombohedral structure that is stable at low temperatures (< ? 10 °C). The formation of the rhombohedral KNbO₃ structure can be explained by the presence of the K⁺ vacancies in the specimen. The KNbO₃ single crystal with an orthorhombic structure formed when the K_2-mNb₂O_6-m/2 single crystal was annealed at 800 °C with 20 wt% of K₂CO₃.     

Properties and crystallization kinetics of low temperature co-fired Li<Subscript>2</Subscript>O-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> electroceramics

The glass-ceramic in the Li₂O-Al₂O₃-SiO₂ system has been prepared by melt quenching route. The crystallization kinetics was studied by differential scanning calorimetry. The effects of sintering temperature on the phase transformation, sintering behavior, bulk density, microstructure, thermal expansion, bending strength and dielectric properties were also investigated by X-ray diffractometry and scanning electron microscopy. (Li, Mg, Zn)_1.7Al₂O₄Si₆O₁₂ is the first crystalline phase forming in the glass-ceramic and transforms to LiAlSi₃O₈ phase at 800 °C. The other two crystalline phases of ZrO₂ and CaMgSi₂O₆ precipitate at 700 and 750 °C, respectively. The densification of this LAS glass-ceramic starts at around 730 °C and stops at about 805 °C. The coefficient of thermal expansion increases with the increasing sintering temperature. The sample sintered at 800 °C for 30 min exhibited excellent properties. The nonisothermal activation energy of crystallization is 149 kJ/mol and the values of Avrami constant (n) are in the range of 3.2 to 3.9. The LAS glass-ceramic sintered at 800 °C for 30 min showed excellent properties. This makes that this material suitable for a number of LTCC applications.     

Microelectrodes for local conductivity and degradation measurements on Al stabilized Li<Subscript>7</Subscript>La<Subscript>3</Subscript>Zr<Subscript>2</Subscript>O<Subscript>12</Subscript> garnets

The attractiveness of Li₇La₃Zr₂O₁₂ (LLZO) cubic based garnets lies in their high ionic conductivity and the combination of thermal and electrochemical stability. However, relations between composition and conductivity as well as degradation effects are still not completely understood. In this contribution we demonstrate the applicability of microelectrodes (Ø = 20–300 μm) for electrochemical impedance spectroscopy (EIS) studies on LLZO garnets. Microelectrodes allow to obtain local information on the ionic conductivity. A comparison between the overall performance of the sample (3.3 × 10^?4 S cm^?1) and local measurements revealed differences in conductivity with a maximum of the locally measured values of 6.3 × 10^?4 S cm^?1 and a minimum of 2.6 × 10^?4 S cm^?1. One reason behind these conductivity variations is most probably a compositional gradient in the sample. In addition, microelectrodes are very sensitive to conductivity changes near to the surface. This was used to investigate the effect of moisture in ambient air on the conductivity variations of LLZO. Substantial changes of the measured Li-ion transport resistance were found, particularly for smaller microelectrodes which probe sample volumes close to the surface.     

Multiferroic,magnetoelectric and magneto-impedance properties of NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript>/(Pb,Sr) TiO<Subscript>3</Subscript> bilayer films

We prepared NiFe₂O₄/(Pb, Sr)TiO₃ (NFO/PST) bilayer films by the chemical solution method and investigated their multiferroic, magnetoelectric and magneto-impedance properties. Multiferroic properties have been observed at room temperature. The bilayer films exhibit saturation polarization P _s ? 26.6 μC/cm² and saturation magnetization M _s ? 134 emu/cm³. With increasing Sr content, M _s. and P _s values of the NFO/PST bilayer films decrease. The variation may be ascribed to the influence of interfacial strain and decrease in tetragonality. High magnetoelectric coupling effect has been observed in the NFO/PST bilayer films with maximum value of α _E  = 6.35 Vcm^?1 Oe^?1 measured at H _DC  ~ 1 kOe and f ~ 10 kHz for Sr ~ 10% (NFO/PST10). The magneto-impedance measurements establish a strong dependence on magnetic field, further confirming magnetoelectric response in NFO/PST bilayer films. An alternative approach for impedance analysis of NFO/PST10 bilayer film provides direct evidence of strain mediated magnetoelectric coupling at room temperature. The results indicate that NFO/PST bilayer films can be considered as a potential multiferroic magnetoelectric material.     

Analysis of domain structure in the Ce<Subscript>0.8</Subscript>Sm<Subscript>0.15</Subscript>Ca<Subscript>0.05</Subscript>O<Subscript>1.875</Subscript> sample

A Ce_0.8Sm_0.15Ca_0.05O_1.875 (S15C05DC) sample is synthesized by a solid-state reaction serving as a potential electrolyte material for intermediate-temperature solid oxide fuel cells. The sintered sample was found to be dense with a cubic fluorite structure. The addition of Ca²⁺ can act as a CeO₂ sintering aid for accelerating the process. The microstructures and properties of the sample were analyzed by X-ray diffractometry, Raman spectroscopy, scanning electron microscopy, thermomechanical analysis, and transmission electron microscopy. Existing oxygen vacancies in the sample are indicated by a Raman peak at 558 cm^?1. The thermal expansion coefficient of the S15C05DC sample at 200–800 °C is approximately 12–14 × 10^?6 °C^?1. The control of domain size is an important factor for improving the conductivity of S15C05DC. Local clustered nano-domains, with higher Sm₂O₃ concentrations, were found to regularly arrange to induce the formation of a nanoscale C-type superlattice structure. While Ca doping decreased the formation of the C-type Sm₂O₃ structure.     

Mechanical and electrical properties of Bi<Subscript>1.5-x</Subscript>La<Subscript>x</Subscript>Zn<Subscript>0.92</Subscript>Nb<Subscript>1.5</Subscript>O<Subscript>6.92</Subscript> pyrochlore ceramics

BiFeO₃-Pb(Mg_1/3Nb_2/3)O₃-PbTiO₃ (BF-PMN-PT) ternary ceramics with pure perovskite phase were prepared through a two-step solid reaction method. Based on structural analysis, the ternary phase diagram of BF-PMN-PT solid solution at room temperature has been established. The Curie temperature T_C, remnant polarization P_r and piezoelectric constant d₃₃ vary in the range of 138 to 225 °C, 15.12 to 23.65 μC/cm² and 129 to 276 pC/N, respectively. The coercive field Ec increases gradually from 5.77 to 29.56 kV/cm upon PT content increasing. The magnetic study suggests that the magnetism turns from diamagnetism for PMN-PT to paramagnetism for BF-PMN-PT by adding BiFeO₃ into PMN-PT and adding more content of BF does not change the paramagnetism further.     

Optimization of the thermoelectric properties of Bi<Subscript>2</Subscript>O<Subscript>2</Subscript>Se ceramics by altering the temperature of spark plasma sintering

The n-type polycrystalline Bi₂O₂Se ceramics were fabricated by solid state reaction and SPSed at different temperatures (873–973 K). The grains of the sample grow up gradually and the grain size enlarges from about 200 nm to micrometer level with the increase of sintering temperature. The highest electrical conductivity of 6.23 S/cm is obtained for the sample sintered at 898 K which benefits from grain orientation along (00l) plane and the highest measured density. The electrical transport properties tend to decline with further increase of the sintering temperature due to the decrease of density and the orientation degree. The maximum power factor of 78.39 μWK^?2m^?1 is obtained at 773 K. The thermal conductivity is intrinsically suppressed owing to the layered crystal structure of Bi₂O₂Se and fine grains within the nanometer size. The ZT value reaches 0.09 at 773 K for the sample SPSed at 898 K and the optimal temperature during the SPS process has been determined.     

Structural,dielectric and magnetic properties of particulate composites of relaxor (BaTi<Subscript>0.85</Subscript>Sn<Subscript>0.15</Subscript>O<Subscript>3</Subscript>) and ferrite (NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript>) synthesized by gel-combustion method

Particulate composites of (1-x) BaTi_0.85Sn_0.15O₃ – x NiFe₂O₄ (with x?=?5, 10,15 and 20 wt%) were synthesized using the solid-state reaction method by sintering at 1350 °C for 4 h. Formation of the diphase composites was confirmed by X-ray diffraction (XRD) and Fourier Transform Infra-red (FTIR) techniques. Temperature (RT-200 °C) and frequency (20 Hz- 1 MHz) dependent of AC conductivity, dielectric constant and dissipation have been studied. The dielectric constant exhibits strong frequency dispersion in the range 20 Hz-1 kHz which is attributed to Maxwell-Wagner interfacial polarization occurring at grain-grain-boundaries interface/interface of grains of BTS-NF. The M-H curve of all the composites exhibited a hysteresis loops typical charcateistic of a ferromagnetic material. The ferromagnetic ordering in the composites on account of NiFe₂O₄ as a constituent is explained using bound magnetic polarons (BMPs) model. The experimental magnetic data have been fitted to BMP model. Value of M_s is smaller, whereas of H_c and M_r are higher of the composites compared to value for NiFe₂O₄. The temperature at which divergence in the M vs. T plot in ZFC and FC starts is higher for the composites than for NiFe₂O₄.     

The Similar Defect Chemistry of Highly-Doped SrBi<Subscript>2</Subscript>Ta<Subscript>2</Subscript>O<Subscript>9</Subscript> and SrBi<Subscript>2</Subscript>Nb<Subscript>2</Subscript>O<Subscript>9</Subscript>

The equilibrium electrical conductivities of undoped SrBi₂Ta₂O₉ (SBT) and SrBi₂Nb₂O₉ (SBN) have been shown to behave quite differently. SBT has the behavior expected for a 1% acceptor-doped oxide, while SBN behaves like a 1% donor-doped oxide. This difference has been related to the substantial cation place exchange that occurs between the Bi^{+ 3} and Sr^{+ 2} ions in the alternating layers of the structure. It was proposed that this place exchange is not entirely self-compensating, as would be expected for a simple, isotropic oxide, but that there is some local compensation within each layer by lattice and/or electronic defects. It is now shown that the equilibrium conductivity of 3% donor-doped SBT is similar to that of undoped SBN, while the equilibrium conductivity of 3% acceptor-doped SBN resembles that of undoped SBT. Thus the defect chemistrys of the two compounds are quite similar, but the equilibrium conductivities are displaced along a doping axis.     

Phase transition,microstructure and properties of (Na<Subscript>0.5</Subscript>Bi<Subscript>0.5</Subscript>)<Subscript>1-x</Subscript>Ba<Subscript>x</Subscript>TiO<Subscript>3</Subscript> lead-free piezoelectric ceramics

In this article, (Na_0.5Bi_0.5)_1-xBa_xTiO₃ lead-free piezoelectric ceramics were prepared by solid-state reaction. The influence of Ba contents on phase structures, compositional distribution and electrical properties of (Na_0.5Bi_0.5)_1-xBa_xTiO₃ ceramics were systematically investigated to further understand the nature of phase transition. It was found that the phase structure of (Na_0.5Bi_0.5)_1-xBa_xTiO₃ transforms from rhombohedral to tetragonal symmetry at x = 0.06 ~ 0.07 and Ba²⁺ segregation forms the coexistence of Ba-rich tetragonal and Ba-deficient rhombohedral phases close to MPB. The electrical properties of prepared samples regularly changed with Ba content, which is closely related to the distribution of rhombohedral and tetragonal phases. The prepared sample near MPB exhibited the largest dielectric constant and the excellent piezoelectric properties (the maximal measuring field reached 78 kV/cm and the piezoelectric constant d ₃₃ = 151pC/N).     

Ionic conduction and crystal structure of aluminum doped NASICON-type LiGe<Subscript>2</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript> glass-ceramic crystallized at different times and temperatures

In this communication, NASICON-type glass-ceramic (lithium germanium phosphate, LiGe₂(PO₄)₃) was prepared as lithium super ionic conductor using aluminum as dopant for ionic conduction improvement. The solid solution was Li_1?+?xAl_xGe_2-x(PO₄)₃ (x?=?0.5) that Ge⁴⁺ ions were partially substituted by Al³⁺ ions in crystal structure. Initial glasses were converted to glass-ceramics at different times and temperatures for maximum ionic conduction achievement. The crystals were characterized by X-ray Diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM), Energy-Dispersive X-ray spectroscopy (EDX), Differential Scanning Calorimetry (DSC) and Complex Impedance Spectroscopy (CIS) methods. The maximum lithium ion conductivity for glass-ceramic, 5.32?×?10^?3 S/cm at 26 °C was obtained for specimen crystallized at 850 °C for 8 h with minimum activation energy of 0.286 eV. Increasing the crystallization temperature results in secondary phase formation in grain boundary and increasing in crystallization time results in microcracks formation in specimen. Both phenomena decreased the ionic conductivity.     

Feasibility of in vivo three-dimensional T<Stack><Subscript>2</Subscript><Superscript>*</Superscript></Stack> mapping using dicarboxy-PROXYL and CW-EPR-based single-point imaging

Objectives

The aim of this study was to demonstrate the feasibility of in vivo three-dimensional (3D) relaxation time T ₂ ^* mapping of a dicarboxy-PROXYL radical using continuous-wave electron paramagnetic resonance (CW-EPR) imaging.

Materials and methods

Isotopically substituted dicarboxy-PROXYL radicals, 3,4-dicarboxy-2,2,5,5-tetra(²H₃)methylpyrrolidin-(3,4-²H₂)-(1-¹⁵N)-1-oxyl (²H,¹⁵N-DCP) and 3,4-dicarboxy-2,2,5,5-tetra(²H₃)methylpyrrolidin-(3,4-²H₂)-1-oxyl (²H-DCP), were used in the study. A clonogenic cell survival assay was performed with the ²H-DCP radical using squamous cell carcinoma (SCC VII) cells. The time course of EPR signal intensities of intravenously injected ²H,¹⁵N-DCP and ²H-DCP radicals were determined in tumor-bearing hind legs of mice (C3H/HeJ, male, n = 5). CW-EPR-based single-point imaging (SPI) was performed for 3D T ₂ ^* mapping.

Results

²H-DCP radical did not exhibit cytotoxicity at concentrations below 10 mM. The in vivo half-life of ²H,¹⁵N-DCP in tumor tissues was 24.7 ± 2.9 min (mean ± standard deviation [SD], n = 5). The in vivo time course of the EPR signal intensity of the ²H,¹⁵N-DCP radical showed a plateau of 10.2 ± 1.2 min (mean ± SD) where the EPR signal intensity remained at more than 90% of the maximum intensity. During the plateau, in vivo 3D T ₂ ^* maps with ²H,¹⁵N-DCP were obtained from tumor-bearing hind legs, with a total acquisition time of 7.5 min.

Conclusion

EPR signals of ²H,¹⁵N-DCP persisted long enough after bolus intravenous injection to conduct in vivo 3D T ₂ ^* mapping with CW-EPR-based SPI.

     

Self-assembly and hydrothermal technique syntheized Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>-RGO nanocomposite: The enhancement effect of electrochemical simultaneous detection of honokiol and magnolol

The nanocomposite of Fe₂O₃-reduced graphene oxide (Fe₂O₃-RGO) was synthesized by a hydrothermal reduction using self-assembly of Fe(OH)₃ colloidal suspension and graphene oxide (GO) as precursors at 180°C. The resulting composites were characterized using XRD, SEM, FTIR, and TGA, and then were used to modify the glassy carbon electrode (GCE). After optimizing the parameters, the electrochemical behavior of honokiol and magnolol on different types of electrode was compared, which indicated that the Fe₂O₃-RGO composite-modified GCE enhanced electrochemical catalysis effect on the simultaneous determination of honokiol and magnolol. In pH 6.4 PBS solution, two well-shaped oxidation peaks at 0.51 and 0.64 V were observed at the Fe₂O₃-RGO composite-modified GCE and two well-shaped oxidation peaks were separated absolutely, which eliminated the disturbance between them. A sensitive and simple electrochemical method was proposed for the simultaneous determination of honokiol and magnolol. As to honokiol, the calibration curve is from 1.5 × 10^?8 ~ 3.3 × 10^?5 M, and the detection limit is 9.64 × 10^?9 M. For magnolol, the linear range is from 7.5 × 10^?8 ~ 2.6 × 10^?5 M, and the detection limit is 1.05 × 10^?8 M.     

Dielectric properties of pure and Mn-doped CaCu<Subscript>3</Subscript>Ti<Subscript>4</Subscript>O<Subscript>12</Subscript> ceramics over a wide temperature range

The effect of manganese doping on the dielectric properties of CaCu₃Ti_4-xMn_xO₁₂ (x?=?0, 0.02, 0.04) were investigated over a broad temperature range (93–723 K) in the frequency range from 100 Hz to 10 MHz. Two dielectric relaxations and two dielectric anomalies were observed. The low-temperature relaxation appearing in the temperature range below 200 K is the characteristic relaxation for CaCu₃Ti₄O₁₂. This relaxation was attributed to the polaron relaxation due to electron hopping between Ti³⁺ and Ti⁴⁺ states. Due to the negative factors of notable decreases in the Ti³⁺/Ti⁴⁺ and Cu³⁺/Cu²⁺ ratios and the concentration of oxygen vacancies as revealed by X-ray photoemission spectroscopy, Mn-doping was found to gradually destroy rather than move this relaxation to a higher temperature. The high-temperature relaxation occurring around room temperature was found to be a Maxwell-Wagner relaxation caused by grain boundaries. Our results confirm that the colossal dielectric behavior in the tested samples results from both polaron and Maxwell-Wagner relaxations, but is predominated by the latter relaxation. The low-temperature anomaly behaves as a phase-transition-like behavior. It was argued to be created by oxygen vacancies transition from static disorder to dynamic disorder. The high-temperature anomaly is an artificial effect caused by negative capacitance.     

Microwave dielectric properties of Na<Superscript>+</Superscript> and M<Superscript>3+</Superscript>-doped Ba(Mg<Subscript>0.5</Subscript>W<Subscript>0.5</Subscript>)O<Subscript>3</Subscript> ceramics

In this study, phase evolution, microstructure, and microwave dielectric properties of (Ba_0.98Na_0.02)(Mg_0.48M³⁺_0.02W_0.5)O₃ (M³⁺?=?Al, Ga, Sc, In, Yb, Y, Dy, Gd, and Sm) ceramics sintered at 1700 °C for 1 h were investigated. All the compounds exhibited an ordered cubic perovskite structure. Regardless of the ionic radius of the doped M³⁺ ions, BaWO₄ was detected as the secondary phase in all the compounds. The field emission scanning electron microscopy (FE-SEM) images revealed a dense microstructure in all the compounds, except in the Al-doped compound, which exhibited an insufficient grain growth. The large and irregularly shaped grains indicated that the liquid phase sintering occurred. Splitting of the A_1g(O) mode was observed in the Raman spectra of large M³⁺ ion-doped compounds. Splitting of the F_2g modes did not occur and the bands were sharp, indicating that the cubic symmetry was retained. As the ionic radius of the doped M³⁺ ions increased, the dielectric constant (ε_r) increased slightly. The compounds doped with M³⁺?=?Sc, In, Yb, and Y exhibited a very high quality factor (Q?×?f₀) in the range of 250,000 ~ 280,000 GHz. In the case of the compounds doped with M³⁺?=?Al, Ga, Sc, In, Yb, Y, and Dy, the value of the temperature coefficient of resonant frequency (τ_f) was in the range of ?24 ~ ?19 ppm/°C, while the Gd and Sm-doped compounds exhibited positive values of 2.8 and 31.2 ppm/°C, respectively. The dielectric constant, quality factor, and temperature coefficient of resonant frequency of the In-doped compound, i.e., (Ba_0.98Na_0.02)(Mg_0.48In_0.02W_0.5)O₃, were 18.7, 286,557 GHz, and???24.4 ppm/°C, respectively.     

Structure and properties of Bi<Subscript>2</Subscript>O<Subscript>3</Subscript> doped Bi(Mg<Subscript>1/2</Subscript>Ti<Subscript>1/2</Subscript>)O<Subscript>3</Subscript>-0.38PbTiO<Subscript>3</Subscript> ceramics with MPB composition

0.62Bi(Mg_1/2Ti_1/2)O₃-0.38PbTiO₃-xwt%Bi₂O₃ (BMT-0.38PT-xBi₂O₃) ceramics were prepared by conventional powder-processing method. It indicated that the morphotropic phase boundary (MPB) region located in 0.0?≤?x?≤?0.3. For x?=?0.3, it exhibited good piezoelectric properties, d₃₃ ~245pC/N and k_p ~40 %. With the increase of Bi₂O₃ content, the Curie temperature (T_c) was found to increase, and the dielectric loss was found to decrease above 200 °C compared with BMT-0.38PT sample. Finally, it can be found that depolarization temperature was around 350 °C by thermal depoling method.     

Influence of fillers on the re-crystallization and dielectric properties of 60ZnO-30B<Subscript>2</Subscript>O<Subscript>3</Subscript>-10SiO<Subscript>2</Subscript> glass

This paper reports re-crystallization behaviour of 60ZnO-30B₂O₃-10SiO₂ pure glass. Influence of different fillers on the re-crystallization is also highlighted. Irrespective of the nature of the filler, glass transition temperature (T_g) remains the same as that of the pure glass at 570 °C. The onset crystallization temperature is enhanced by 15 to 25 °C owing to filler addition. The peak crystallization temperature corresponding to Zn₃B₂O₆, ZnB₂O₄ and willemite occurs at 735, 810 and 851 °C for the pure glass. In the presence of alumina, gahnite emerges first at 700 °C followed by ZnB₂O₄ phase. With mullite as filler, initially ZnB₂O₄ and willemite formed at 700 °C and gahnite phase emerged only at 750 °C and peaks at 787 °C. In the presence of fused silica only ZnB₂O₄ and willemite phases were observed. The dielectric properties of the pure glass and that of the glass + fillers are also reported. Re-crystallization of various low K phases ensures good dielectric porpertis with reduced glass content after sintenring.     

Crystallization,microstructures and properties of low temperature co-fired CaO-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> glass-ceramic

CaO-Al₂O₃-SiO₂ glass-ceramic were prepared by melt quenching technique. The crystallization behavior and properties were studied by means of a non-isothermal, thermal analysis technique, X-ray diffraction and scanning electron microscopy. The influence of sintering temperature on phase formation, microstructure, bending strength, dielectric and thermal properties were determined. The activation energy of crystallization and the Avrami parameter were also discussed. The X-ray diffraction results show that SiO₂ phase could be found in all samples and CaSiO₃ and anorthite phases could only be observed in the samples sintered at above 875°C. The densification of glass-ceramic starts at 730°C after the liquid glass is formed and stops at 803°C. Complete densification was achieved at 875°C and the highest mechanical strength was obtained at 850°C, but density significantly decreased at higher temperatures. The coefficient of thermal expansion and the dielectric constant increase with the increasing sintering temperature. The value of the Avrami parameter (n) is ~1.6 and the apparent activation energy (E) is 298 kJ/mol.