Reactive sintering mechanism of Ti + Mo<Subscript>2</Subscript>C and Ti + VC powder compacts

TiC reinforced Ti-matrix composites have been synthesized successfully by reactive sintering of Ti-1.5%Fe-2.25%Mo (wt%) powder compacts with addition of Mo₂C and VC particles. The reactions for the formation of TiC particles start at 600 °C, but the distribution of TiC particles and the densification behavior in the two compacts are significantly influenced by the metal carbides (Mo₂C or VC). The compact with addition of Mo₂C has a relative density of 98% after sintering at 1300 °C for 1.5 h, but TiC particles are agglomerated in the Ti matrix. The compact with addition of VC has a relative density of about 91% after sintering at 1300 °C for 1.5 h, but TiC particles distribute more homogenously in the Ti matrix. Different TiC particle distribution and densification behaviors are attributed to the reaction rates between Ti and metal carbides and the subsequent diffusion process.     

Effects of addition of bismuth oxide and glass on the properties of lithium ferrite for ferrimagnetic pastes

Lithium ferrite, Li_0.5Fe_2.5O₄, has been prepared by decomposition of organometallic complexes at 800° C, and the optimization of heating schedule for conversion into ferrite has been studied. The effects of addition of glass, essential for adhesion of the ferrite film to alumina substrates, and bismuth oxide, as a sintering aid, on the properties and densification of lithium ferrite have been examined. X-ray diffraction, electron probe micro analysis (EPMA) and scanning electron microscopy (SEM) techniques have been used to study the solubility and distribution of bismuth oxide, grain growth and pore morphology. It has been found that the addition of bismuth oxide (up to 1.5 wt%) improves densification and increases resistivity of the lithium ferrite but the addition of glass causes a reduction of the resistivity. Although bismuth oxide forms a solid solution, it is not uniformly distributed throughout the ferrite phase. It is shown that the addition of bismuth oxide improves the insertion loss in microwave devices fabricated using ferrimagnetic pastes.     

The effects of silica content,sintering temperature and sintering time on a Ni‐Zn ferrite

Abstract

In this experiment the effects of silica content, sintering time, and sintering temperature on the microstructure and magnetic properties of a ferrite, Ni₀₃₂Zn₀₆₈Fe₂O₄, were studied.

The initial permeability is reduced only slightly when the silica content is less than 0.2 wt %. The Q value is proportional to the silica content approximately. The peak value of μ _iQ product is about constant when the silica content is less than 0.2 wt %.

The best sintering temperature is between 1175°C and 1200°C. The addition of silica (<0.2 wt%) enhances the rate of densification, but the control of sintering time has to be more precise because the addition of silica makes the shape of μ _iQ product peak become sharper and narrower.     

Effect of crystallizable glass addition on sintering and dielectric behaviors of barium titanate ceramics

A crystallizable glass which can precipitate barium titanate was added to BaTiO₃ ceramics to study its effect on sintering behavior and dielectric properties of the composites. High densification (>95 % theoretical density) was achieved by addition of glass phase and the dielectric constant of composites was enhanced through the crystallization of glass phase. A composite with 90 wt% BaTiO₃ and 10 wt% glass showed a dielectric constant of ~2,300 at room temperature at 1 kHz and a dielectric breakdown strength about 140 kV/cm.     

Effect of lithium magnesium zinc borosilicate glass addition on densification temperature and dielectric properties of Mg<Subscript>2</Subscript>SiO<Subscript>4</Subscript> ceramics

Mg₂SiO₄ (Forsterite) ceramics were synthesized by solid state route. The effect of lithium magnesium zinc borosilicate (LMZBS) glass addition on the densification temperature and microwave dielectric properties of forsterite ceramics was investigated. The crystal structure and microstructure of ceramic–glass composites were studied by X-ray diffraction and scanning electron microscopic techniques. The dielectric properties of the sintered samples were measured in the microwave frequency range by the resonance method. Addition of 0.5 wt% LMZBS glass improved densification with ε _r = 7.3 and Qxf = 121,200 GHz. Addition of 15 wt% LMZBS glass lowered the sintering temperature to about 950 °C with ε _r = 6.75 and Qxf = 30,600 GHz. The reactivity of 15 wt% LMZBS glass added forsterite with silver was also studied. The result shows that forsterite doped with suitable amount of LMZBS glass is a possible material for LTCC and microwave substrate applications.     

Low-temperature sintering of Z-type hexagonal ferrite by addition of fluorine containing glass powder

In order to reduce the sintering temperature of Ba₃Co₂Fe₂₄O₄₁ (Co₂Z), fluorine containing glass powder was added as a sintering aid to ferrite powder with a Co₂Z stoichiometric composition prepared by a solid-state reaction, and dense sintered specimens could be obtained at 1000°C in air. The densification was achieved by liquid-phase sintering which was induced by the melting of the additive glass at 800°C. The main crystalline phase was Co₂Z, and spinel ferrite appeared as the impurity phase. By sintering in a sealed container, the densification was accelerated still more, and in addition to spinel ferrite, Ba-M also appeared as the impurity phase. The Ba-M contained some Co instead of Fe, and grew to discontinuously large hexagonal plate-like grains. In a fluorine and/or fluorides rich atmosphere, Co₂Z was discomposed to Ba-M and spinel ferrite, and large hexagonal plate-like grains appeared. These results suggest that fluorine and/or fluorides evaporated from the additive glass decomposed Co₂Z to Ba-M and spinel ferrite, and induced the discontinuously grain growth of Ba-M. The initial permeability was lower than that of the specimen with no additive glass but remained almost constant in the frequency regions up to 1 GHz.     

Electrical behavior of Gd-doped CeO2 electrolyte ceramics sintered from nanopowders prepared by mechanical alloying process

The densification behavior of nanocrystalline Gd-doped ceria electrolyte, synthesized via mechanical alloying process, was investigated by means of the conventional pressure less sintering and the two-step sintering methods. The effect of the heating rate and the amounts of dopant on the sinterability of Ce_1−x Gd _x O_(2−δ) x = 0.2 (2GDC) and x = 0.3 (3GDC) oxides was studied, which indicated that the gadolinium retards densification and grain growth in the final state of the conventional sintering and 2GDC samples reach 94% density at 1,550 °C. Subsequent investigation on the grain growth in the fully densified ceramics showed that lowering of the heating rate and increasing of the soaking time reduce the effect of dopant and cause samples to be densified to the higher theoretical density (97%) at lower temperatures (1,400 °C). Fully dense Gd-doped ceria ceramics with finest grain size (900–1,100 nm) can be obtained by two-step sintering method. Electrical conductivity measurement in the GDC samples was studied by impedance spectroscopy. The grain boundary conductivity in these specimens obtained by two-step sintering method was compared with normal sintered specimens. It is concluded that the reduced conductivity observed in the two-step sintering specimen is attributable to the microstructure changes obtained by increased of grain boundary resistivity.     

Pressureless sintering and characterization of cordierite/ZrO2 composites

Cordierite/ZrO₂ composites with 5 to 25 wt% ZrO₂ were fabricated by conventional powder mixing and pressureless sintering method. Their densification behavior, microstructure, mechanical and thermal properties were studied. By dispersing 25 wt% (9.57 vol%) ZrO₂, densified cordierite/ZrO₂ composite with a relative density of 98.5% was obtained at an optimum sintering condition of 1440 °C and 2 h. ZrO₂ particles were homogenously dispersed within matrix grains and at the grain boundaries. The intragranular particles were finer than 100 nm and the intergranular particles were coarser. Both fracture strength and toughness could be enhanced more than two times higher, compare to those of monolithic cordierite, by dispersing 25 wt% ZrO₂ into the cordierite matrix. The toughening mechanism in the present composites was mainly attributed to martensitic transformation due to ZrO₂ dispersion. Electronic Publication     

On the sintering kinetics of titania doped ceramic lanthanum chromite

The sintering behaviour of lanthanum chromite with the addition of 1 to 3 wt% TiO₂ was studied. Densification was examined as a function of sintering temperature and TiO₂ concentration. The results showed that pure LaCrO₃ could not be densified to >75% of the theoretical density, while the densities exceeding 90% of the theoretical were achieved with 3 wt% titania addition at 1600° C. Metallographic study reveals a normal grain growth following the rate equationD ²−D ₀ ² =kt. Activation energies both for densification and grain growth have been estimated to be ≈ (80±5) k cal/mole in case of 3 wt% TiO₂ addition.     

Effects of SrO–B2O3–SiO2 glass additive on the microstructure and dielectric properties of CaCu3Ti4O12

The effect of SrO–B₂O₃–SiO₂ glass additive (SBS) on the microstructure and dielectric properties of CaCu₃Ti₄O₁₂ (CCTO) ceramics was investigated. This SBS–added CCTO ceramics were prepared by the solid state reaction. The undesirable impurity phases Ca₃SiO₅ started appearing in the XRD patterns, suggesting a possible chemical reaction between CaTiO₃ and SiO₂ (the devitrification production of SBS glass). The SBS glass additive promoted the grain growth and densification of CCTO ceramics. Cole–Cole plots of conductance suggested that the resistivity grain boundary decreased with increasing amount of SBS glass (when x = 0–2 wt%), then increased (when x = 2–3 wt%). The addition of SBS glass was desirable to increase the dielectric constants (up to 10⁴) and lowered the dielectric losses of CCTO over the frequency range of 450–40 kHz at the relatively lower sintering temperature for relatively shorter sintering time (1,050 °C, 12 h).     

Effect of metal oxide precursor on sintering shrinkage, microstructure evolution and electrical properties of silver-based pastes

Since the shrinkage behavior of silver-based films has been correlated with the characteristics of oxide additives used, the relative role of metal oxides and metal-organic precursors in sintering shrinkage and microstructure evolution of silver films was investigated and compared in this work. Films with an oxide powder additive exhibit two-stage shrinkage behavior in contrast to one-stage continuous shrinkage, which occurs in silver films with metal-organic precursors, added. Furthermore, metal-organic precursors are less effective than metal oxide powders in reducing shrinkage of silver-based films. That can be reasonably explained that metal-organic precursors can be effectively decorated around silver powder to inhibit the sintering densification. The Zr-based organic precursor among the metal-organic precursors exhibits optimal retardation in sintering densification of silver film, which is probably interrelated to refractory characteristics of ZrO₂. The unique conductivity and grain growth of silver film with 1.0 wt% tungsten-organic precursor added was possibly due to the partial dissolution of W into Ag.     

Preparation and characterization of ZrB2-SiC ultra-high temperature ceramics by microwave sintering

ZrB₂-SiC ultra-high temperature ceramic composites reinforced by nano-SiC whiskers and SiC particles were prepared by microwave sintering at 1850°C. XRD and SEM techniques were used to characterize the sintered samples. It was found that microwave sintering can promote the densification of the composites at lower temperatures. The addition of SiC also improved the densification of ZrB₂-SiC composites and almost fully dense ZrB₂-SiC composites were obtained when the amount of SiC increased up to 30vol.%. Flexural strength and fracture toughness of the ZrB₂-SiC composites were also enhanced; the maximum strength and toughness reached 625 MPa and 7.18 MPa·m^1/2, respectively.     

Preparation and characterization of ZrB<Subscript>2</Subscript>-SiC ultra-high temperature ceramics by microwave sintering

ZrB₂-SiC ultra-high temperature ceramic composites reinforced by nano-SiC whiskers and SiC particles were prepared by microwave sintering at 1850°C. XRD and SEM techniques were used to characterize the sintered samples. It was found that microwave sintering can promote the densification of the composites at lower temperatures. The addition of SiC also improved the densification of ZrB₂-SiC composites and almost fully dense ZrB₂-SiC composites were obtained when the amount of SiC increased up to 30vol.%. Flexural strength and fracture toughness of the ZrB₂-SiC composites were also enhanced; the maximum strength and toughness reached 625 MPa and 7.18 MPa·m^1/2, respectively.     

The sintering of combustion-synthesized titanium diboride

A comparative study of the sinterability of combustion-synthesized titanium diboride was conducted over the temperature range of 1800 to 2100° C. During the initia! sintering stage, the densification rate was slightly higher in the combustion-synthesized than in the commercially obtained titanium diboride. For sintering times of > 30 min, however, the shrinkage rates for both types of powders were the same. The activation energy for the late sintering stage was 774 ± 46 kJ mol^–1, consistent with 8 volume diffusion mechanism, end was the same for both combustion-synthesized and commercial powders. The microstructures of sintered specimens with initial particle size below 1O µm exhibited a grain size ranging from 5 to over 40 µm after 30 min of sintering. The addition of 5 wt% NbB₂ to the combustion-synthesized resulted in enhanced shrinkage during the initial sintering stage, but did not affect later stage kinetics. Various amounts of additives of CrB₂, NiB and TiC had no effect on early and late stage sintering kinetics, with the exception of 50 wt% TiC which appreciably inhibited densification.     

Stress sensitivity of inductance in NiMgCuZn ferrites and development of a stress insensitive ferrite composition for microinductors

Three series of NiMgCuZn ferrites were prepared by conventional sintering process. The formation of single phase in these ferrites was confirmed by x-ray diffraction. Initial permeability measurements on these samples were carried out in the temperature range of 30–400°C. The effect of the external applied stress on the open magnetic circuit type coil with these ferrites was studied by applying uniaxial compressive stress parallel to magnetizing direction and the change in the inductance was measured. The variation of ratio of inductance (ΔL/L)% increases upto certain applied compressive stress and there after it decreases, showing different stress sensitivities for different compositions of ferrites studied in the present work. With a view to develop stress insensitive NiMgCuZn ferrite, a low stress sensitivity composition among all the ferrites studied was chosen and different amounts of SiO₂ were added to it and a series of ferrite compositions were prepared. The variation of ratio of inductance (ΔL/L)% with external applied compressive stress was examined. These results show that, 0.05 wt% SiO₂ added Ni_0.3Mg_0.3Cu_0.1Zn_0.3Fe₂O₄ ferrite exhibited stress insensitivity. It was noticed that addition of SiO₂ was found to be effective in reducing the stress sensitivity. This was confirmed from the elastic behaviour studies at room temperature on these ferrite samples. These studies were carried out to develop a ferrite composition for its use as core material for microinductor applications.     

Effect of BiVO4 doping on the magnetic properties and microstructure of NiCuZn ferrites

Effects of BiVO₄ addition on the microstructural development and magnetic properties of a NiCuZn ferrite were investigated by conventional solid state reaction method. For the low temperature sintering (<961 °C), 0–2 wt% of BiVO₄ was added to the ferrites. The grain size and bulk density gradually increased with the increase in the BiVO₄ content and more uniform and compact structure at 1.0 wt% BiVO₄ were obtained. The permeability decreases gradually with increase in BiVO₄ content BiVO₄ doped in NiCuZn ferrites improved magnetic properties and reduced the magnetic loss tangent. The samples may be excellent candidates to fabricate multilayer chip inductors and LTCC passive devices.     

Electrochemical behavior of sintered YAG dispersed 316L stainless steel composites

The present work investigates the effect of second phase dispersoid addition and sintering temperature on the corrosion behavior of austenitic (316L) stainless steels. Yttrium aluminum garnet (YAG) was added as second phase to the austenitic stainless steels in varying amounts (1, 2.5 and 7.5 wt.%), and the compacts were sintered at 1200 and 1400 °C corresponding to solid-state and supersolidus sintering, respectively. The sintered samples were characterized for their corrosion resistance in 0.1N H₂SO₄ using potentiodynamic polarization. It is shown that YAG addition does not appreciably increase corrosion rate of 316L compacts. However, as compared to solid-state sintering, supersolidus sintering resulted in superior corrosion resistance. The electrochemical behavior of the 316L–YAG composites with sintering temperature is correlated to the densification response and microstructure.     

Sintering mechanism of fine zirconia powders with alumina added by powder mixing and chemical processes

The present study examined the sintering behavior of fine zirconia powders (containing 2.9 mol% Y₂O₃) with and without small amounts of Al₂O₃ added by different ways: powder mixing (PM), homogeneous precipitation (HP), and hydrolysis of alkoxide (HA). The initial sintering behavior was examined by both measurement methods of a constant rate of heating and isothermal shrinkage. In the PM process, Al₂O₃ particles pinned the shrinkage of zirconia powder compact at the initial stage and diffuse toward zirconia surface to enhance the sintering. This initial sintering mechanism was explained by the grain-boundary diffusion for the Al₂O₃-free powder and the volume diffusion for Al₂O₃-added powder. When Al₂O₃ was added to zirconia powder by HP and HA processes, the densification rate was more stimulated compared to the PM process. The initial sintering mechanism did not change by the way for Al₂O₃ addition. The Al₂O₃ addition by chemical processes of HP and HA tended to enhance the grain growth of zirconia, while the uniform microstructure was achieved because of homogeneous addition of Al₂O₃ by those processes.     

Investigation on addition of ZrO2-3 mol% Y2O3 powder on sintering behavior and mechanical properties of B4C

The effect of ZrO₂-3% Y₂O₃ addition on densification, sintering behavior and mechanical properties of a boron carbide matrix was investigated. When adding 0–30 wt% of ZrO₂-3% Y₂O₃ to B₄C sintered densities were increased from 75% to 98.5%. Sinterability was significantly improved by addition of a small amount of ZrO₂-3% Y₂O₃. As a result of density improvement, mechanical properties such as hardness, strength and fracture toughness were increased remarkably. However, when the amount of ZrO₂-3% Y₂O₃ exceed from 20 wt%. Hardness started to reduce.     

Fabrication and properties of YBa2Cu3O7-δAg composite superconducting wires by plastic extrusion technique

YBa₂Cu₃O_7-δ (Y123)-Ag composite superconducting wires were fabricated by the plastic extrusion method which involves plastic paste making, die extrusion, binder burn-out and the firing process. The as-extruded Y123-Ag wires were so flexible that they can be easily fabricated into a desirable shape. The current-carrying properties of the wire are dependent on sample size, sintering temperature and silver content. The critical current density, J _c, of the Y123 wire with a large cross-section was lower than that of the wires with a small cross-section, probably due to the large self-induced magnetic field. J _c of the Y123-Ag wires increased with increasing sintering temperature but abruptly decreased above 910 °C, which is close to the eutectic temperature of the Y–Ba–Cu–O system. A silver addition of 10–20 wt% slightly increased J _c of the Y123 (at 77 K and 0 T, it was 140 and 250 A cm ^-2 for the undoped Y123 wire and the Y123 wire with 20 wt% Ag addition, respectively), but further silver addition had a deleterious effect on J _c (180 A cm ^-2 for 30 wt% Ag addition). The small increment in J _c in the Y123 wire with 10–20 wt% Ag addition appears to be due to the enhanced densification and the associated microstructural variation. The decreased J _c of the Y123 wire with 30 wt% Ag addition is considered to be due to the formation of non-superconducting phase, Y₂BaCuO₅ (Y211), BaCuO₂ and CuO phases via the decomposition of the Y123 phase. This revised version was published online in November 2006 with corrections to the Cover Date.