Hot-pressed ceramic SiC–YAG materials

Dense SiC-based ceramic materials containing yttrium aluminum garnet (YAG) as an oxide sintering aid have been prepared by hot pressing in the temperature range 1750–1850°C. As a result of melting, the oxides fill spaces between the SiC particles, contributing to the densification of the material and mass transport during the hot pressing process. The present results demonstrate that relatively small amounts of the oxides (≤5 wt %) are needed to ensure a high degree of densification of the SiC–YAG materials. The best physicomechanical properties are offered by the SiC + 3 wt % YAG material sintered at a temperature of 1850°C: ρ = 3.24 ± 0.01 g/cm³, П = 1.1 ± 0.1%, σ_b = 640 ± 10 MPa; K_Ic = 6.4 ± 0.2 MPa m^1/2, Еel = 410 ± 20 GPa, and HV = 26.0 ± 0.2 GPa. This material experiences predominantly intercrystalline fracture.     

Sintering and electromagnetic properties of BaFe12O19 ferrite prepared by co-precipitation method

BaFe₁₂O₁₉ (BaM) was synthesized through the co-precipitation route. Pure phase BaM was formed after calcination of precipitated powder at 900 °C. BaM was sintered at three different temperatures; 1100, 1200, and 1300 °C to study the sintering kinetics by varying the sintering time from 1 to 4 h. Apparent porosity decreased, and bulk density increased with increasing sintering temperature and period. A bulk density of about 4.6 g/cm³ was achieved after sintering at 1300 °C/4 h. The rate-controlling mechanism of BaM densification was the diffusion of oxygen, and the activation energy for the sintering process was 274 kJ/mol. The grain size of BaM increased with rising sintering temperatures. Permittivity increased from about 11 to 17 and the permeability increased from about 10 to 16 with the increase in sintering temperature from 1100 to 1300 °C. Saturation magnetization was also enhanced to about 69 emu/g after sintering at 1300 °C/4 h. Therefore, BaM ferrite synthesized through the co-precipitation route can be effectively used for high-frequency applications after sintering at 1300 °C.

     

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.     

Spark plasma sintering of a p-type Si1?x Ge x alloy: identification of the densification mechanism by isothermal and anisothermal methods

Spark plasma sintering of a p-type Si_0.795Ge_0.200B_0.005 alloy has been investigated in vacuum, in the 400–1200 °C temperature range. The densification mechanism has been determined using isothermal and anisothermal methods. In spite of a slight material degradation for the highest sintering temperatures (occurrence of cristobalite nodules homogeneously dispersed in intergranular and intragranular positions), it is proposed that densification proceeds by grain boundary sliding accommodated most probably by silicon volume diffusion. The microstructure observation of several sintered samples using transmission electron microscopy supports the densification mechanism advanced. Because the elemental grains remain mostly equiaxe whatever the sintering conditions, a grain intercalation mechanism may be also implicated during densification.     

Novel microwave assisted synthesis of highly doped phase pure Nd:YAG nanopowder

For the first time, the studies on 2 to 10 at.% neodymium (Nd³⁺) ion doped Yttrium Aluminum Garnet (Nd:YAG) nanopowders obtained by microwave assisted citrate nitrate gel combustion synthesis is described in this work. This paper reports on high doping of Nd³⁺ ions with retaining the cubic garnet structure of YAG as evidenced from XRD, except the case of 8 at.% doped Nd:YAG. Phase pure YAG formation with 8 at.% Nd³⁺ doping was explored by using urea and alanine as alternative to citric acid complexing agents. Complete crystallization of YAG as a result of 2 hour thermal treatment at 900 °C under oxygen supply was studied by using Fourier Transform Infra-Red Spectroscopy (FTIR) and X-Ray Diffraction (XRD) techniques. With an increase in the dopant concentration a red shift in the FTIR peaks was observed. Using the XRD data, the cell parameter of Nd³⁺ (2 to 6 and 10 at.%) YAG was found to increase with an increase in the dopant concentration. The average primary particle size calculated using Scherrer’s equation was ～25 nm which was additionally supported by Transmission Electron Microscopy (TEM) results yielding particle sizes in the range of ～25 to 30 nm for all the cases.     

Preparation of YAG gel coated ZrB2–SiC composite prepared by gelcasting and pressureless sintering

In this paper, gelcasting and pressureless sintering of YAG gel coated ZrB₂–SiC (YZS) composite were conducted. YAG gel coated ZrB₂–SiC (YZS) suspension was firstly prepared through sol–gel route. Poly (acrylic acid) was used as dispersant. YZS suspension had the lowest viscosity when using 0.6 wt.% PAA as dispersant. Gelcasting was conducted based on AM–MBAM system. The gelcast YZS sample was then pressureless sintered to about 97% density. During sintering, YAG promoted the densification process from solid state sintering to liquid phase sintering. The average grain sizes of ZrB₂ and SiC in the YZS composite were 3.8 and 1.3 μm, respectively. The flexural strength, fracture toughness and microhardness were 375 ± 37 MPa, 4.13 ± 0.45 MPa m^1/2 and 14.1 ± 0.5 GPa, respectively.     

Influence of laser wavelength and beam profile on Nd:YAG laser assisted formation of polycrystalline-Si films

Influence of wavelengths and beam profiles of a pulsed Nd³⁺:YAG laser on the formation of a polycrystalline-silicon (poly-Si) on a-Si thin film is investigated. Two sets of samples of amorphous-Silicon (a-Si) thin films deposited on glass (a-Si/glass) and crystalline Si (a-Si/c-Si) substrates were treated with different laser-fluence values. After the laser treatment, the films were analyzed by a scanning electron microscope, the Raman spectroscopy technique and the resistance-measurement technique. In the case of the third harmonics (355 nm) of the Nd³⁺:YAG laser, poly-Si films were obtained with laser-fluence values ranging from 260 mJ/cm² to 560 mJ/cm², where as in the case of the second harmonics (532 nm), the process window for the formation of poly-Si films, in terms of the laser fluence, was ranging from 300 mJ/cm² to 480 mJ/cm². On the other hand, in the case of samples treated with the fundamental wavelength (1064 nm), a narrow process window with higher laser-fluence values around 1100 mJ/cm² was observed. Further, the substrate was also affected because of the higher laser-fluence value. It has also been observed that the crystallization characteristics of poly-Si films improved with the flat-top intensity distribution as compared to the Gaussian intensity distribution of the Nd³⁺:YAG laser beam. A theoretical simulation based on thermal modeling was performed to understand the mechanism of crystallization.     

Effect of heating mode and temperature on sintering of YAG dispersed 434L ferritic stainless steel

This study examines the effect of heating mode, sintering temperature, and varying yttria alumina garnet (YAG) addition (5 and 10 wt%) on the densification and properties of ferritic (434L) stainless steel. The straight 434L stainless steel and 434L–YAG composites were sintered in a conventional and a 2.45 GHz microwave furnace. The composites were sintered to solid-state as well as supersolidus sintering temperature at 1200 and 1400 °C, respectively. Both 434L and 434L–YAG compacts coupled with microwaves and underwent rapid heating (∼45 °C/min). This resulted in about 85% reduction in the processing time. For all compositions microwave sintering results in greater densification. As compared to conventional sintering, microwave sintered compacts exhibit a more refined microstructure, thereby, resulting in higher bulk hardness. The mechanical properties and sliding wear resistance of 434L stainless steel is shown to be sensitive both to the sintering condition as well as YAG addition and has been correlated to the effect of heating mode on the pore morphology.     

Y<Subscript>2</Subscript>O<Subscript>3</Subscript> and Nd<Subscript>2</Subscript>O<Subscript>3</Subscript> co-stabilized ZrO<Subscript>2</Subscript>-WC composites

Y₂O₃ + Nd₂O₃ co-stabilized ZrO₂-based composites with 40 vol% WC were fully densified by pulsed electric current sintering (PECS) at 1350 °C and 1450 °C. The influence of the PECS temperature and Nd₂O₃ co-stabilizer content on the densification, hardness, fracture toughness and bending strength of the composites was investigated. The best combination of properties was obtained for a 1 mol% Y₂O₃ and 0.75 mol% Nd₂O₃ co-stabilized composite densified for 2 min at 1450 °C under a pressure of 62 MPa, resulting in a hardness of 15.5 ± 0.2 GPa, an excellent toughness of 9.6 ± 0.4 MPa.m^0.5 and an impressive 3-point bending strength of 2.04 ± 0.08 GPa. The hydrothermal stability of the 1 mol% Y₂O₃ + 1 mol% Nd₂O₃ co-stabilized ZrO₂-WC (60/40) composites was compared with that of the equivalent 2 mol% Y₂O₃ stabilized ceramic. The double stabilized composite did not degrade in 1.5 MPa steam at 200 °C after 4000 min, whereas the yttria stabilized composite degraded after less than 2000 min. Moreover, the (1Y,1Nd) ZrO₂-WC composites have a substantially higher toughness (~9 MPa.m^0.5) than their 2Y stabilized equivalents (~7 MPa.m^0.5).     

Two-step sintering and electrical properties of sol–gel derived 0.94(Bi<Subscript>0.5</Subscript>Na<Subscript>0.5</Subscript>)TiO<Subscript>3</Subscript>–0.06BaTiO<Subscript>3</Subscript> lead-free ceramics

Two-step pressureless sintering of sol–gel derived 0.94(Bi_0.5Na_0.5)TiO₃–0.06BaTiO₃ (BNT-BT) lead-free piezoelectric ceramics were investigated in comparison with conventional sintering. The effect of sintering regimes on the densification, grain growth behavior and electrical properties was discussed in detail. The results indicated that BNT-BT ceramics with a density of 95%, a relatively fine grain size of 850 nm and comparable piezoelectric properties (d₃₃ ~170 pC/N, k_p ~0.26, Q_m ~102) had been achieved by pre-sintering at 1,150 °C to reach a critical density of 78%, and then cooling to a lower temperature of 1,050 °C for 20 h. The critical density value proves important at which the grain boundary diffusion could be maintained but the grain boundary migration suppressed at the same time. Moreover, the volatilization loss of Bi and Na elements could be inhibited by two-step sintering. Both the reduction of the grain size and the inhibition of the stoichiometry deviation together account for the variation of various electrical properties.     

Sintering of Fe-doped Bi0.5Na0.5TiO3 at < 1000 °C

Fe-doped Bi_0.5Na_0.5TiO₃ ceramics with Fe-ion content varied from 0 to 0.15 at.% were successfully prepared by conventional solid state reaction method. The sintering temperature used was between 850 and 1000 °C. X-ray diffraction patterns showed that all produced ceramics were single phase with a rhombohedral structure. SEM micrographs of the ceramics showed a dramatic change in densification behavior as a result of Fe-ion doping. At 850 °C, the undoped BNT ceramic had a very porous structure. As the Fe-ion concentration increased, the ceramics showed denser microstructures and, for the sample containing 0.15 at.% Fe, a very dense grain structure with almost no porosity was obtained. This microstructural observation agreed well with the measured density whose value increased with increasing Fe content. The relative density of at least 95% was achieved in 0.15 at.% Fe-doped BNT ceramics even when it was sintered at 850 °C. Increasing the sintering temperature only had an effect of increasing the grain size of this sample without appreciably affecting its density. The results of this investigation showed that addition of Fe₂O₃ in BNT could help improve the densification process and significantly reduced the sintering temperature of BNT ceramics.     

Constitutive modeling of alumina sintering: grain-size effect on dominant densification mechanism

In the present work, alumina powders with the initial grain sizes of 0.9 and 7.0 μm, respectively, were sintered at different temperatures. Constitutive laws for densification were employed to model the sintering process of alumina ceramics. Based on the constitutive laws employed and the experimental results obtained, the dominant densification mechanism was identified and the effect of grain size on dominant densification mechanism was discussed. The activation energy for densification was also evaluated. In the investigated sintering temperature range, interface reaction was identified as the controlling process in sintering of alumina powders with the initial grain size of 0.9 μm, while grain-boundary diffusion was identified as the dominant process in sintering of alumina powders with the initial grain size of 7.0 μm. The activation energies for densification of the finer and coarser grain size alumina ceramics were determined as 342 and 384 kJ mol⁻¹, respectively, which provided a strong support on the densification mechanism investigation.     

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.     

Strategies for low-temperature sintering of BST ceramics with attractive dielectric properties

In this study, the powders of the Ba_0.75Sr_0.25TiO₃ (BST) nanoparticles were directly synthesized by milling of Ba(OH)₂·8H₂O, Sr(OH)₂·8H₂O, and Ti(BuO)₄ in ethanol at room temperature. They have homogenous grains of?~?15 nm and high sintering activity. The dense ceramics with the density?>?90% can be obtained at a sintering temperature of?≤?950 °C by adding 3 wt% sintering aids of Bi₂O₃ and Li₂CO₃. Several Bi-related intermediate compounds act as perovskite-structured templates to sintering the ceramics at a different temperature. They enhance the mass transfer and promote the sintering densification. These compounds such as Ba₂BiO₄ and SrBiO₄ appear at 800 °C, LiBa₄Bi₃O₁₁ and Sr_1.2Bi_0.8O₃ appear over 830 °C, and Bi_8.11Ba_0.89O_13.05 appears at 950 °C. The cation Bi in them can have mixture valences of 3+ and 5+. It makes the ceramics as semiconducting state with the dark gray color and decreases the ceramic resistivities. With the sintering temperature increase, especially at 950 °C, the cation Bi tends back to single valence of +3 in the ceramics. The most of alkaline earth cations in Bi-related compounds will release and resorb into the lattice of BST and drive the sintering densification. The BST ceramics can have a peak dielectric constant?>?6500 (at 53 °C) with loss?<?0.025 at 10 kHz, and resistivity?>?10¹² Ω cm when sintered at a temperature of?≥?900 °C with 3 wt% sintering aids. They have a potential application for multiple layer ceramic capacitors (MLCC) with silver inner electrodes.

     

Doubly Q-switched tape casting YAG/Nd:YAG/YAG ceramic laser

A doubly Q-switched 1.06 μm pulsed laser using a novel tape casting YAG/Nd:YAG/YAG composite ceramic with a sandwich structure was demonstrated for the first time. Compared to purely acousto-optical (AO) Q-switching, this laser using an AO Q-switch and Cr⁴⁺:YAG saturable absorber simultaneously can generate shorter pulses. The pulsed laser performance was investigated at two modulated repetition rates of 10 and 20 kHz.     

Ce dopant segregation in Y3Al5O12 optical ceramics

Ce³⁺-doped YAG garnet optical ceramic have been sintered at the Shanghai Institute of Ceramics in China to characterize dopant distribution in optical ceramics by combining optical spectroscopy and two spatially resolved techniques as imaging confocal microscopy and transmission electron microscopy. A strong Ce³⁺ segregation and spatial variations of content between grains and grain boundaries has been confirmed by quantitative data obtained by TEM microscopy. This observation is another evidence of the inhomogeneous Ce³⁺ distribution across grain and grain boundaries in optical ceramics comparable to that of Nd³⁺ ions in YAG ceramics. These results correlate well with low segregation coefficients of Nd³⁺ and Ce³⁺ observed in the garnet crystals grown from the melt and/or flux.     

Low-temperature sintering mechanism on uranium dioxide

Based on a point defect model, the mechanism of low-temperature sintering of uranium dioxide was studied in this paper. The diffusion coefficient of uranium in UO_{2 + x}, sintering temperature and densification equation in low-temperature sintering were analyzed by both the point defect model and low-temperature sintering experiments. The results showed that the diffusion activation energy of uranium in over-stoichiometric UO_{2 + x} was lowered by 3.0 ev than that in stoichiometric UO₂. And the diffusion coefficient of uranium in UO_{2 + x} was proportional to x². In addition, the theoretical low temperature sintering temperature was calculated to be in the range of 1089–1151 °C, which indicated that it was necessary to maintain proper over-stoichiometric oxygen for low-temperature sintering process. Moreover, the calculation results by the point defect model matched perfectly with the experiment results, PDM might be a good model to describe the relationships between defects concentration and atmosphere composition.     

Study on the sintering mechanism of KNN-based lead-free piezoelectric ceramics

The sintering process and mechanism of (K, Na, Li) (Nb, Ta, Sb)O₃ (KNLNTS) solid solution were investigated. The results show that the KNLNTS forms via the reaction of A₂CO₃(A: K,Na,Li) and B₂O₅(B: Nb,Ta,Sb) at 400–800 °C. The kinetics for the formation of KNLNTS during solid-state reaction is investigated using an isothermal method. Based on the reaction kinetic isothermal analysis, KNLNTS formation is corroborated as being controlled by diffusion mechanism. It has been found that sintering densification occurs within a narrow temperature range, and the density decreases apparently when the sintering temperature slightly exceeds the optimal one. Abnormal grain growth tends to occur after reaching the maximum density and get intensified with increasing temperature. The effect of sintering temperature and time on the shrinkage of powder compacts during sintering were studied. The sintering process in the KNLNTS solid solutions may be explained by the grain boundary diffusion model inferring from the shrinkage rate of about 0.3.     

Sintering and characterization of YAG dispersed ferritic stainless steels

The present study investigates the effect of yttrium aluminium garnet (YAG) addition on the densification, mechanical, tribological and corrosion behaviour of ferritic (434L) stainless steels. The composites were sintered at both solid-state (1200 °C) and supersolidus (1400 °C) sintering conditions. Supersolidus sintering results in superior densification, hardness and corrosion resistance of both straight 434L stainless steel as well as YAG reinforced 434L stainless steels. The addition of YAG to 434L stainless steels at supersolidus sintered conditions improves the strength and wear resistance of 434L stainless steels without significantly degrading the corrosion performance.     

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.