Highly transparent yttrium titanate (Y2Ti2O7) ceramics from co-precipitated powders

Highly transparent yttrium titanate (Y₂Ti₂O₇) ceramics were fabricated by vacuum sintering using co-precipitated powders for the first time. The effects of the powder calcination temperature on the phase composition, morphology of the calcined powders, and on the microstructure and transmittance of the Y₂Ti₂O₇ ceramics were investigated. When the calcination temperature was above 850 °C, pure phase Y₂Ti₂O₇ nanopowders with high sintering activity were obtained. Transparent Y₂Ti₂O₇ ceramics were obtained after vacuum sintered at 1600 °C for 6 h and annealed at 1100 °C for 5 h in air. The highest transmittance reached 73% at 1000 nm when the calcination temperature was 1150 °C. The measured refractive index of Y₂Ti₂O₇ ceramics was higher than 2.24 at the wavelength range of 350–1000 nm, making it a promising candidate for optical devices.     

Preparation and study of the mechanical and optical properties of infrared transparent Y2O3–MgO composite ceramics

In this study, fine Y₂O₃–MgO composite nanopowders were synthesized via the sol–gel method. Dense Y₂O₃–MgO composite ceramics were fabricated by pre-sintering the green body in air at different temperatures for 1 h and then subjecting the sintered bodies to hot isostatic pressing at 1300°C for 1 h. The effects of pre-sintering temperature on the microstructural, mechanical, and optical properties of the resulting ceramics were studied. The average grain size of the ceramics was increased, whereas their hardness and fracture toughness were decreased with increasing pre-sintering temperature. A maximum fracture toughness of 1.42 MPa·m^1/2 and Vickers hardness of 10.4 GPa were obtained. The average flexural strength of the ceramics was 411 MPa at room temperature and reached 361 MPa at 600°C. A transmittance of 84% in the 3–5 µm region was obtained when the composite ceramics were sintered at 1400°C. Moreover, a transmittance of 76% in the 3–5 µm region was obtained at 500°C.     

A novel approach of synthesizing nano Y2O3 powders for the fabrication of submicron IR transparent ceramics

A facile methodology of synthesizing highly reactive, round-edged, Sulfur–free nano Y₂O₃ powders to fabricate submicron IR transparent yttria ceramics having a unique combination of superior optical and mechanical properties are reported for the first time. Dispersion of yttrium hydroxide into aqueous sol and addition of seed particles produced near-spherical yttria powders having non – aggregated particles with narrow size distribution. The powder exhibited excellent sinterability reaching near-theoretical density at temperatures around 1400 °C in air. Effective inter-particle coordination and traces of Al additives assisted achieving superior densification. Sintered specimens showed average grain sizes closer to 700 nm. Post-sinter hot isostatic pressing eliminated the residual porosity from the sintered samples leading to exhibit IR transmissions up to 84% in the 2.0–9.0 μm regions, equivalent to single crystal Y₂O₃. Achieving densification through solid-state sintering and retaining the sintered grain sizes in the submicron regions significantly enhanced the mechanical properties. Sintered and HIPed Y₂O₃ specimens were further characterized for their thermal properties at temperature regions between ambient to 950 °C.     

Low-loss YIG thick films for microwave applications

We report the fabrication, densification and characterization of polycrystalline free-standing yttrium iron garnet Y₃Fe₅O₁₂ (YIG) thick films in this paper. The thick films were fabricated using a double doctor blade technique from co-precipitated nanocrystalline YIG powders. The sintering temperature of YIG thick films was varied from 1000 to 1400°C. A volume diffusion mechanism is seen to govern the densification process. A high relative density of ~99% could be achieved in a YIG thick film, with a thickness of 80?µm, sintered at a relatively low temperature of 1300?°C. The magnetization value ~1750?Oe, near to the YIG bulk magnetization value and an acceptable low ferromagnetic resonance (FMR) linewidth (?H) of 80?Oe resulted in these high density YIG thick films with microwave device possibilities.     

Effects of Gd Substitution on Sintering and Optical Properties of Highly Transparent (Y0.95−xGdxEu0.05)2O3 Ceramics

Highly transparent (Y_0.95?xGd_xEu_0.05)₂O₃ (x = 0.15–0.55) ceramics have been fabricated by vacuum sintering at the relatively low temperature of 1700°C for 4 h with the in‐line transmittances of 73.6%–79.5% at the Eu³⁺ emission wavelength of 613 nm (~91.9%–99.3% of the theoretical transmittance of Y_1.34Gd_0.6Eu_0.06O₃ single crystal), whereas the x = 0.65 ceramic undergoes a phase transformation at 1650°C and has a transparency of 53.4% at the lower sintering temperature of 1625°C. The effects of Gd³⁺ substitution for Y³⁺ on the particle characteristics, sintering kinetics, and optical performances of the materials were systematically studied. The results show that (1) calcining the layered rare‐earth hydroxide precursors of the ternary Y–Gd–Eu system yielded rounded oxide particles with greatly reduced hard agglomeration and the particle/crystallite size slightly decreases along with increasing Gd³⁺ incorporation; (2) in the temperature range 1100°C–1480°C, the sintering kinetics of (Y_0.95?xGd_xEu_0.05)₂O₃ is mainly controlled by grain‐boundary diffusion with similar activation energies of ~230 kJ/mol; (3) Gd³⁺ addition promotes grain growth and densification in the temperature range 1100°C–1400°C; (4) the bandgap energies of the (Y_0.95?xGd_xEu_0.05)₂O₃ ceramics generally decrease with increasing x; however, they are much lower than those of the oxide powders; (5) both the oxide powders and the transparent ceramics exhibit the typical red emission of Eu³⁺ at ~613 nm (the ⁵D₀→⁷F₂ transition) under charge transfer (CT) excitation. Gd³⁺ incorporation enhances the photoluminescence and shortens the fluorescence lifetime of Eu³⁺.     

Formation peculiarities and optical properties of highly-doped (Y0.86La0.09Yb0.05)2O3 transparent ceramics

Formation peculiarities of highly-doped (Y_0.86La_0.09Yb_0.05)₂O₃ transparent ceramics have been studied by X-ray diffraction and electron microscopy methods. The phase composition evolution of 1.81Y₂O₃∙0.18La₂O₃∙0.01Yb₂O₃ powder mixtures annealed at the temperatures of 1100, 1200, 1300, and 1400 °C has been studied by XRD. It has been shown that Yb₂O₃ phase dissolves in Y₂O₃ matrix in the calcination temperature range of 1300–1400 °C. Complete dissolution of La₂O₃ in Y₂O₃ matrix occurs at temperatures above 1400 °C. La³⁺ ions enter in Y₂O₃ and Yb₂O₃ crystal structures simultaneously in the 1200–1300 °C range, which leads to a remarkable increase in the volume of the corresponding crystal lattices. The possible reasons for suppressing the crystalline growth of Y₂O₃ and Yb₂O₃ cubic phases have been discussed. Finally, (Y_0.86La_0.09Yb_0.05)₂O₃ transparent ceramics have been obtained by solid-state vacuum sintering at 1650–1750 °C. Ceramics synthesized at a temperature of 1750 °C have been characterized by an in-line optical transmittance of 60% and a homogeneous distribution of constituent components within the volume and along the grain boundaries.     

Effects of Sintering Temperature on Open‐Volume Defects and Thermoluminescence of Yttria and Lutetia Ceramics

The effects of different processing steps and processing conditions for the fabrication of Y₂O₃ and Lu₂O₃ ceramics were investigated, particularly the effects of calcination, and sintering temperature on the content of open‐volume and electronic defects. Ceramic bodies were prepared from calcined powders by sintering from 1400°C to 1700°C for 20 h. Density was determined by the Archimedes method and showed pellets reached about 99% of Y₂O₃ density for temperatures ≥1450°C, and reached 98% for sintering at 1700°C for Lu₂O₃. The content of open‐volume defects was followed by positron annihilation lifetime (PAL) measurements. For both materials, two lifetimes were obtained. The faster lifetime, 211 ps for Y₂O₃ and 204 ps for Lu₂O₃, was assigned to bulk annihilation with possible contribution of grain boundaries. The longer lifetime was assigned to positronium annihilation in open‐volume defects with radii of 2–4 Å. Doppler broadening analysis revealed the same type of defect in Lu₂O₃ ceramics for all sintering temperatures. PAL analysis results showed that densification was achieved through the elimination and agglomeration of open‐volume defects. Thermoluminescence (TL) measurements of Y₂O₃ showed that sintering is beneficial in eliminating traps and/or recombination centers, and that higher sintering temperatures increase TL signal.     

Potential of the Sinter-HIP-technique for the Development of High-temperature Resistant Si3N4-ceramics

Silicon nitride ceramics were densified with the sintering additives Y₂O₃ and SiO₂ by a two-step sinter-HIP-process. Three compositions with additive contents between 2 and 7 wt% Y₂O₃ were prepared to study the influence of the processing conditions on the mechanical properties. The minimum additive content required for nearly complete densification (>98.5%) was only 2 wt% Y₂O₃. However, densification was limited to certain Y₂O₃/SiO₂ ratios. The additive-rich samples revealed a mean strength at room temperature up to 800 MPa which degrades at 1400°C. The material with only 2 wt% Y₂O₃ has a room temperature strength of ∼500 MPa, but no strength degradation up to 1400°C. The lower strength correlates with a pronounced increase in brittleness with a decreasing additive content indicated by a fracture toughness of only 2·5 MPam^1/2 for composition 2/0. The investigated materials exhibit a relatively high creep resistance at 1400°C with creep rates down to 1·5×10⁻⁹ s⁻¹.     

Densification of nanocrystalline Y2O3 ceramic powder by spark plasma sintering

Nanocrystalline Y₂O₃ powders with 18 nm crystallite size were sintered using spark plasma sintering (SPS) at different conditions between 1100 and 1600 °C. Dense specimens were fabricated at 100 MPa and 1400 °C for 5 min duration. A maximum in density was observed at 1400 °C. The grain size continuously increased with the SPS temperature into the micrometer size range. The maximum in density arises from competition between densification and grain growth. Retarded densification above 1400 °C is associated with enhanced grain growth that resulted in residual pores within the grains. Analysis of the grain growth kinetics resulted in activation energy of 150 kJ mol^?1 and associated diffusion coefficients higher by 10³ than expected for Y³⁺ grain boundary diffusion. The enhanced diffusion may be explained by combined surface diffusion and particle coarsening during the heating up with grain boundary diffusion at the SPS temperature.     

Ultrafine-grained β-Sialon fabricated by two-stage sintering and study on diffusion toughening of Ti–22Al–25Nb

The ultrafine-grained β-Sialon ceramics were fabricated by spark plasma sintering at different temperatures with inorganic Al₂O₃–Y₂O₃ and Ti–22Al–25Nb intermetallic powder as composite additives. The research showed that β-Sialon ceramics achieve two-stage sintering densification. Al₂O₃–Y₂O₃ inorganic additives promoted the synthesis and densification of β-Sialon ceramics at 1125–1215°C. Ti–22Al–25Nb intermetallic powder diffused Ti and Nb elements at 1240–1425°C, thereby improving the fracture toughness of β-Sialon ceramics. The maximum fracture toughness (∼9.69 MPa m^1/2) under 19.6 N was obtained for β-Sialon ceramics sintered at 1600°C.     

Synthesis of BaCeO3 and BaCe0.9Y0.1O3−δ from mixed oxalate precursors

An oxalate precipitation route is proposed for the synthesis of BaCe_1−xY_xO₃ (x = 0 and 0.1) after calcination at 1100 °C. The precipitation temperature (70 °C) was a determinant parameter for producing a pure perovskite phase after calcination at 1100 °C for 1 h. TG/DTA measurements showed that the co-precipitated (Ba, Ce and Y) oxalate had a different thermal behaviour from single oxalates. Despite a simple grinding procedure, sintered BaCe_0.9Y_0.1O_3−δ pellets (1400 °C, 48 h) presented 90.7% of relative density and preliminary impedance measurements showed an overall conductivity of around 2 × 10⁻⁴ S cm⁻¹ at 320 °C.     

Effects of Ho3+ concentration on the fabrication and properties of Ho: Y2O3-MgO nanocomposite for Mid-infrared laser applications

Infrared transparent Ho: Y₂O₃-MgO nanocomposite ceramics with a volume ratio of 50:50 (RE₂O₃: MgO) were prepared by combining sol-gel powder synthesis and hot-pressing sintering techniques. In order to obtain Ho: Y₂O₃-MgO nanocomposite ceramics with fine grain size, dense microstructure and homogeneous phase domains, the effect of sintering temperature and Ho³⁺ doping concentration were studied. Transmittance and SEM measurement revealed that the grain size of 3 at.% Ho: Y₂O₃-MgO ceramic sintered at 1250 °C is 141 nm, and the transmission is up to 85.2% at 5 μm. The detailed spectroscopic investigation of x at.% Ho: Y₂O₃-MgO (x = 1, 3, 5, 7, 9, 15) ceramics was performed. The nanocomposites exhibited photoluminescence properties similar to that of Ho: Y₂O₃ crystals and ceramics. In addition, the thermal conductivity of 3 at.% Ho: Y₂O₃-MgO ceramic is 13.04 W/m·K, which is superior to that of Ho:Y₂O₃ ceramics. The high transmission, excellent thermal conductivity, and outstanding optical characteristics indicated that Ho: Y₂O₃-MgO ceramics is a promising material for efficient infrared solid-state laser.     

Significant improvement of resistance to dry/water oxygen corrosion at medium and high temperatures of SiC/SiC composites upon matrix modification by Ca-Y-Al-Si-O microcrystalline glass

Matrix modification is of great significance for the densification of CVI-SiC/SiC, as well as the improvement of self-healing and oxidation resistance. A eutectic component of Y₂O₃-Al₂O₃-SiO₂ system modified with CaO (CYAS) was used in this study to modify SiC/SiC at 1400 °C. The oxidation behaviour of the composites was investigated under dry/water oxygen atmosphere at 900 °C and 1300 ℃. Compared to the relatively dense SiC/SiC, the modified SiC/SiC showed a slight increase in flexural strength and fracture toughness at room temperature, as well as a significant increase in oxidation resistance and densification. Our work provides a low-cost, simple-to-operate, short-cycle densification method for CVI-SiC/SiC composites that increases their oxidation resistance without compromising their mechanical properties at room temperature.     

Development of optical grade polycrystalline YIG ceramics for faraday rotator

Fully dense and infrared transparent YIG (Y₃Fe₅O₁₂) ceramics was successfully produced by solid‐state reaction of Y₂O₃ and Fe₂O₃ powders. Its relative density reached 99.8% (5.16 g/cm³) after sintered at 1400°C for 3 hours, and almost 100% relative density (5.17 g/cm³) was obtained by additional HIP treatment. It was transparent at wavelength ranges longer than 1100 nm, and its in‐line transmittance (ca. 75%‐77%) was very comparable to that of commercial YIG single crystal especially over 1700 nm. Faraday rotation angle at 1300 and 1550 nm was 224 and 175 deg/cm, respectively, and extinction ratio was 35 dB and insertion loss polarized at 45° was 0.3 dB at 1550 nm. It was confirmed that the Faraday effect of polycrystalline material which has numerous grain boundaries and randomized crystal orientations is analogous to that of the single crystal. To the best of our knowledge, this is the first report to achieve highly transparent polycrystalline iron garnet ceramics successfully, and it is expected to use as an optical isolator in optical communication and medical field.     

Microstructure and properties of SiCf/SiC composite joints with CaO–Y2O3–Al2O3–SiO2 interlayer

Using CaO, Y₂O₃, Al₂O₃, and SiO₂ micron-powders as raw materials, CaO–Y₂O₃–Al₂O₃–SiO₂ (CYAS) glass was prepared using water cooling method. The coefficient of thermal expansion (CTE) of CYAS glass was found to be 4.3 × 10^?6/K, which was similar to that of SiC_f/SiC composites. The glass transition temperature of CYAS glass was determined to be 723.1 °C. With the increase of temperature, CYAS glass powder exhibited crystallization and sintering behaviors. Below 1300 °C, yttrium disilicate, mullite and cristobalite crystals gradually precipitated out. However, above 1300 °C, the crystals started diminishing, eventually disappearing after heat treatment at 1400 °C. CYAS glass powder was used to join SiC_f/SiC composites. The results showed that the joint gradually densified as brazing temperature increased, while the phase in the interlayer was consistent with that of glass powder heated at the same temperature. The holding time had little effect on phase composition of the joint, while longer holding time was more beneficial to the elimination of residual bubbles in the interlayer and promoted the infiltration of glass solder into SiC_f/SiC composites. The joint brazed at 1400 °C/30 min was dense and defect-free with the highest shear strength of about 57.1 MPa.     

Effect of waste-derived MA spinel on sintering and stabilization behavior of partially stabilized double phase zirconia

Cubic-stabilized zirconia ceramic composites have been synthesized by conventional sintering, starting from commercial m-ZrO₂, Y₂O₃, and waste-derived magnesium aluminate spinel (MA) powders. In this work, the effect of sintering temperature and MA content on stabilization and densification properties of YSZ have been duly considered. MA-free YSZ0 composite sintered at 1600°C-1700°C revealed m- and t-ZrO₂ dual-phase structure where its m-ZrO₂ was partially stabilized upon temperature rising into tetragonal phase by Y³⁺ diffusion inside zirconia structure. YSZ10-50 composites containing 10-50 wt% MA demonstrated dissimilar behavior where their m-ZrO₂ was transformed and stabilized into a cubic form by diffusion of Y³⁺, Mg⁺², and Al⁺³ inside zirconia lattice. Furthermore, densification of YSZ10-50 powder mixtures by conventional sintering at 1600°C for 2 hours resulted in fully dense compacts with micrometer-sized grains. The outcomes indicate that MA has a significant effect on m-ZrO₂ stabilization into the cubic phase structure at room temperature. In this respect, this study offers huge potentials for developing fully stabilized c-ZrO₂ ceramics that could be possibly used as industrial ceramics for structural applications of harsh chemical and thermal environmental conditions.     

Synthesis of nanostructured Nd:Y2O3 powders by carbonate-precipitation process for Nd:YAG ceramics

Neodymium doped yttria (Nd:Y₂O₃) nanopowders were synthesized by a co-precipitation method, and the effect of thermal decomposition behavior of the precursors were studied. Nonlinear and linear heating schedules (NHS and LHS) were adopted during the calcination processes. The results show that as compared to the LHS the NHS can not only lower the crystallization temperature substantially, but also decrease the mean particle size and lighten the particle agglomeration in the obtained Nd:Y₂O₃ nanopowders. Using the obtained well-dispersed Nd:Y₂O₃ and commercial Al₂O₃ powders, transparent Nd:YAG ceramics were fabricated at 1750 °C in vacuum. Better transparency can be obtained by using the Nd:Y₂O₃ powders calcined in the NHS instead of the LHS.     

High optical quality Y2O3 transparent ceramics with fine grain size fabricated by low temperature air pre-sintering and post-HIP treatment

High optical quality Y₂O₃ transparent ceramics with fine grain size were successfully fabricated by air pre-sintering at various temperature ranging from 1500 to 1600 °C combined with a post-hot-isostatic pressing (HIP) treatment using co-precipitated powders as the starting material. The fully dense Y₂O₃ transparent ceramic with highest transparency was obtained by pre-sintered at 1550 °C for 4 h in air and post-HIPed at 1600 °C for 3 h (the pressure of HIP 200 MPa), and it had fine microstructure and the average grain size was 0.96 μm. In addition, the in-line transmittance of the ceramic reached 81.7% at 1064 nm (1 mm thickness). By this approach, the transparent Y₂O₃ ceramics with fine grain size (<1.6 μm) were elaborated without any sintering aid.     

Effects of calcination atmosphere on monodispersed spherical particles for highly optical transparent yttria ceramics

Highly sinterable powders are required for the fabrication of transparent ceramics. Here, we studied the effects of calcination atmosphere on the characteristics of monodispersed spherical Y₂O₃ powders, such as crystallite size and particle density, for high optical transparent ceramics. It was found that vacuum calcination around the crystallization temperature is the crucial step to eliminate intragranular pores in the spherical particle. The fast decomposition rate in a vacuum creates smaller crystallites, and the following higher calcination temperature results in the enhancement of pore elimination. The in‐line transmittance of the transparent Y₂O₃ ceramics, vacuum sintered at 1750°C, was improved by increasing the particle density of the as‐calcined powders. This result indicates that the high‐density starting particles effectively enhance the pore elimination during the fabrication of transparent Y₂O₃ ceramics.     

Enhanced mechanical properties of 3 Y2O3 stabilized tetragonal ZrO2 incorporating tourmaline particles

The current study reports on the improvement of mechanical properties of 3?mol% Y₂O₃ stabilized tetragonal ZrO₂ (3Y-TZP) by introduction of tourmaline through ball milling and subsequent densification by pressureless sintering at 800, 1200, 1300, 1400?°C. Findings demonstrate that no matter which sintering temperature the 3Y-TZP ceramic containing 2?wt% tourmaline reach a maximum value in flexural strength and fracture toughness as compared to other composite ceramics. As the tourmaline content is 2?wt% and the sintering temperature is 1300?°C, the flexural strength and fracture toughness of the composite ceramics are the highest, increases of 36.2% and 36.6% over plain 3Y-TZP ceramic respectively. The unique microstructure was systematically investigated through X-ray diffraction, scanning electron microscopy, energy dispersive spectrum, and flourier transform-infrared. The strengthening and toughening mechanism of tourmaline in 3Y-TZP ceramic were also discussed.