Mechanical Properties of Submicrometer‐Grained Transparent Yttria Ceramics by Hot Pressing with Hot‐Isostatic Pressing

Here, we report the fabrication and mechanical properties of submicrometer‐grained (0.29–0.58 μm) transparent yttria ceramics by hot pressing combined with hot‐isostatic pressing. The effects of the grain size on the microhardness and the fracture toughness were studied. An unusual decrease of the fracture toughness with an increase in the grain size was revealed, which may be attributed to the different grain size dependence of the fracture behavior of the ZrO₂‐doped yttria ceramics compared to that of other yttria ceramics. The microhardness and fracture toughness of the transparent yttria ceramics were found to be better than those of the large‐grained yttria ceramics.     

Highly transparent cerium-doped yttria ceramics for full-band UV-shielding window applications

Highly transparent cerium-doped yttria ceramics were fabricated via a pressureless sintering method with an addition of 10 at.% La₂O₃ and 1 at.% ZrO₂ as a binary sintering additive. With an increase in the Ce doping concentration from 0 to 3 at.%, the optical absorption edge of yttria ceramics exhibited a significant red shift from 290 to 380 nm as a result of the 4f–5d transition of Ce³⁺ and the charge transfer of Ce⁴⁺ (i.e., Ce⁴⁺+e^–→Ce³⁺). For a 2-mm thick sample doped with 3 at.% Ce, the total ultraviolet radiation (UV) transmittance (220–400 nm) is only 1.7%, indicating a nearly complete UV absorption. Meanwhile, the specimens possess high in-line transmittance levels in both the visible and the infrared regions (i.e., >70% at 450 nm and ∼80% at 1100 nm). Additionally, the present specimens were confirmed to have good enough mechanical strength levels (∼165 MPa) and thermal conductivity (∼5 W/m·K), which are comparable or even better compared to those of previously reported transparent yttria ceramics. The results of this work indicate that cerium-doped transparent yttria ceramics are promising candidate materials for full-band UV-shielding window applications.     

Enhancement of the optical transmittance of hot-pressed transparent yttria ceramics by a multi-step sintering process

In this work, we report the enhancement of the optical transmittance of yttria ceramics via a ‘pre-sintering/hot-pressing/hot-isostatic pressing’ multi-step process. The in-line transmittance reaches 78.0% at 400 nm and 83.2% at 1100 nm with an average grain size of approximately 1 µm. This sintering route is derived and upgraded from our previously reported one-step hot-pressing method for the fabrication of transparent yttria ceramics. Through the enhanced strength of the green body by pre-sintering, the formation of cracks and the breaking up of the as-hot-pressed samples can be effectively suppressed, leading to sound or crack-free but less transparent samples. After a post-HIPing treatment, the optical transmittance of the samples with a pre-sintering step was substantially improved to higher levels in the visible and the IR wavelengths compared to that of a sample which does not undergo pre-sintering. The corresponding mechanism was revealed by microstructural analyses.     

Transparent and Luminescent ZnS Ceramics Consolidated by Vacuum Hot Pressing Method

In this study, ZnS powders with homogeneous morphology were synthesized using a colloidal processing method. Vacuum hot pressing was subsequently applied to consolidate the ZnS powders into infrared transparent ceramics (77.3% transmittance at wavelengths of 6.74 and 9.29 μm). The phase composition of the sintered ZnS suggests the presence of wurtzite as a minor phase in addition to the primary sphalerite phase, and microstructural analysis indicates that the ceramics are highly densified. It has been found that the VHP‐sintered ZnS ceramics exhibit blue (450 nm) and green (530 nm) luminescence, which is due to the formation of zinc vacancies and sulfur interstitials, respectively, during the sintering process.     

Transparent ZnS Ceramics by Sintering of High Purity Monodisperse Nanopowders

We report an efficient way of preparing transparent ZnS ceramics using the hot‐pressing technique. It has been found that the transparency is highly dependent on the purity and the grain size distribution of the starting ZnS powders. Highly pure and monodisperse ZnS powders have been obtained by posttreatment of the precipitated powders in a H₂S/N₂ flow for 2 h at 600°C. The obtained ZnS ceramics show fully dense and homogeneous microstructure with average grain size of ~1 μm and smooth grain boundaries, leading to an excellent transmission of around 70% in the mid‐ and far‐ IR regions. The preparation technique described in this study is highly reproducible.     

Highly transparent yttria ceramics with Nb2O5/Ta2O5 as novel sintering additives by pressureless vacuum sintering

Highly transparent yttria ceramics were fabricated by pressureless sintering with Nb₂O₅ or Ta₂O₅ as a novel sintering additive. The optical transmittance, microstructural evolution, and thermo-mechanical properties of the samples were investigated. The optimal doping concentrations of Nb₂O₅ and Ta₂O₅ are 0.3 and 0.2 at.%, respectively, which are much lower compared to those of previously reported counterparts. The transmittance of the sample with 0.3 at.% Nb₂O₅ reaches 81.6% at 1100 nm and 72.4% at 400 nm (2 mm in thickness), similar transmittance was obtained in the sample with 0.2 at.% Ta₂O₅. The microhardness (∼7 GPa), fracture toughness (∼0.85 MPa·m^1/2), and biaxial strength (∼200 MPa) of the present samples were confirmed to be comparable or even better compared to those of previously reported transparent yttria ceramics fabricated by pressureless sintering. Furthermore, the present samples, by virtue of the low doping concentrations, possessed relatively high thermal conductivity values (>10 W/m·K), which substantially guaranteed high thermal shock resistance.     

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.     

Fabrication and optical characterizations of Yb,Er codoped CaF2 transparent ceramic

Nanoparticles of Yb, Er codoped calcium fluoride were obtained by a co-precipitation method. Scanning electron microscope (SEM) and X-ray powder diffraction (XRD) analysis showed that the obtained nanoparticles were single fluorite phase with grains size around 30–50 nm. Yb, Er:CaF₂ transparent ceramics were fabricated by hot pressing (HP) the nanoparticles at a temperature of 800 °C in a vacuum environment. For a 2 mm thickness ceramic sample, the transmittance at 1200 nm reached about 83%. Microstructures were characterized using SEM analysis, and the average grain size was about 700 nm. Grain boundaries of the ceramic sample were clean and no impurities were detected. The absorption, upconversion and infrared emission spectra of transparent ceramic sample under 978 nm excitation were measured and discussed.     

Fabrication of Transparent Pb(Mg1/3Nb2/3)O3–PbTiO3 Based Ceramics by Conventional Sintering

Transparent 0.9Pb(Mg_1/3Nb_2/3)O₃–0.1PbTiO₃ (PMN‐PT) based ceramics were prepared by a conventional solid‐state synthesis without using a hot‐press method. The ceramics became transparent when they were sintered in an O₂ atmosphere. The optical transmission increased with decreasing diameter of the calcined powder, which was controlled by the size of zirconia ball‐milling media. Substitution of 3 mol% La for Pb in PMN‐PT further increased the optical transmission to 68% at the wavelength of 2000 nm, which was comparable to that of hot‐pressed Pb(Mg_1/3Nb_2/3)O₃‐PbTiO₃ based transparent ceramics.     

Fabrication of Gd2O3‐MgO nanocomposite optical ceramics with varied crystallographic modifications of Gd2O3 constituent

The fabrication of Gd₂O₃‐MgO nanocomposite optical ceramics via hot‐pressing using sol‐gel derived cubic‐Gd₂O₃ and MgO nanopowders was investigated. The precursor powder calcined at 600°C had an average particle size of 12 nm. The effects of hot‐pressing temperature on constituent phases, microstructure, mid‐infrared transmittance, and microhardness were studied. The crystallographic modifications of Gd₂O₃ phase varied with the increase in sintering temperature from 1250 to 1350°C. The monoclinic‐Gd₂O₃ phase was retained for the composite sintered at 1350°C and the sample had an average grain size of 90 nm, excellent transmission (80.4%‐84.8%) over 3‐6 μm wavelength range, and enhanced hardness value of 14.1 GPa.     

Microstructure and properties characterization of Yb:Lu2O3 transparent ceramics from co-precipitated nano-powders

5at.% Yb:Lu2O3 transparent ceramics were fabricated successfully by vacuum sintering along with hot isostatic pressing posttreatment from the nanopowders. The influences of calcination temperature on morphology and microstructures of powders and ceramics were studied systematically. The optimal ceramic sample from the nanopowder calcined at 1050°C shows uniform and dense microstructure with the in-line transmittance of 81.5% at 1100 nm. The results of the thermal measurements, that is, thermal conductivity and specific heat, were related to the changes occurring in the microstructure of the ceramics studied. It was shown on this basis that appropriate control of the technological process of sintering ceramics makes it possible to obtain laser ceramics with very good thermal properties as well as maintaining their high optical quality. Concerning the laser performance, the highest-optical quality 5at.% Yb:Lu₂O₃ sample was pumped in quasi-continuous wave conditions measuring a maximum output power of 2.59 W with a corresponding slope efficiency of 32.4%.     

Achieving fabrication of highly transparent Y2O3 ceramics via air pre-sintering by deionization treatment of suspension

An easy albeit quite effective deionization suspension treatment was adopted to alleviate the detrimental effects related to the hydrolysis of Y₂O₃ in an aqueous medium. Fabrication of highly transparent Y₂O₃ ceramics with a fine grain size via air pre-sintering and post–hot isostatic pressing (HIP) treatment without using any sintering additive was achieved using the treated suspensions. The hydrolysis issue of Y₂O₃ powder in an aqueous medium was effectively alleviated by using deionization treatment, and a well-dispersed suspension with a low concentration of dissolved Y³⁺ species was obtained. The dispersed suspensions were consolidated by the centrifugal casting method, and the green bodies derived from the suspension of 35.0 vol% solid loading showed an improved homogeneity with a relative density of 52.1%. Fully dense Y₂O₃ transparent ceramic with high transparency was obtained by pre-sintering consolidated green compacts at a low temperature of 1400°C for 16 h in air followed by a post-HIP treatment at 1550°C for 2 h under 200 MPa pressure. The sample had a fine average grain size of 690 nm. The in-line transmittance of the sample reached 83.3% and 81.8% at 1100 nm and 800 nm, respectively, very close to the theoretical values of Y₂O₃.     

Optical Characterizations of Hot‐Pressed Erbium‐Doped Calcium Fluoride Transparent Ceramic

Nanoparticles of erbium‐doped calcium fluoride were synthesised by the coprecipitation method. Micromorphology of the obtained nanoparticles was observed by transmission electron microscopy. The nanoparticles were hot‐pressed in a vacuum environment to achieve Er:CaF₂ transparent ceramic. X‐ray diffraction analysis confirmed the crystallization of a single fluorite phase after sintered. Transmittance spectrum of Er:CaF₂ ceramic sample was measured, and the transmittance at 1200 nm reached about 87%. Microstructures were characterized using field‐emission scanning electron microscopy. The luminescence spectrum of Er:CaF₂ transparent ceramics under 488‐ and 978‐nm excitation was measured and discussed. It was evidenced that strong cross‐relaxation processes between Er³⁺ ions occur at high dopant concentration, and favoring the red emission at the expense of the green one.     

Fabrication and laser operation of Yb:Lu2O3 transparent ceramics from co-precipitated nano-powders

In this article, 5 at.% Yb:Lu₂O₃ transparent ceramics were fabricated by vacuum sintering combined with hot isostatic pressing (HIP) posttreatment using co-precipitated nano-powders. The influence of precipitant molar ratio, ammonium hydrogen carbonate, to metal ions (AHC/M³⁺, R value) on the properties of Yb:Lu₂O₃ precursors and calcined powders was investigated systematically. It was found that the powders with different R value calcined at 1100°C for 4 hours were pure cubic Lu₂O₃ but the morphologies of precursors and powders behaved differently. The opaque samples pre-sintered at 1500°C for 2 hours grew into transparent ceramics after HIP posttreatment at 1750°C for 1 hour. The final ceramic with R = 4.8 showed the best optical quality with the in-line transmittance of 79.7% at 1100 nm. The quasi-CW laser operation was performed at 1034 nm and 1080 nm with a maximum output power up to 8.15 W as well as a corresponding slope efficiency of 58.4%.     

Transparent tetragonal-cubic zirconia composite ceramics densified by spark plasma sintering and hot isostatic pressing

Targeting higher toughness transparent ceramics, tetragonal (3 mol % yttria) and cubic (8 mol % yttria) ZrO₂ starting powder mixtures were densified by spark plasma sintering (SPS) in vacuum at 1100 °C and post hot isostatic pressing (HIP) in argon at 1100 °C. The influence of the ultra-fine microstructure and phase composition on the fracture resistance and light transmission in the visible and infra-red range was assessed. Of special interest was the influence of a thermal annealing step in air on the transparency of the SPS and SPS-HIP ceramics.     

Influence of post-HIP temperature on microstructural and optical properties of pure MgAl2O4 spinel: From opaque to transparent ceramics

Transparent MgAl₂O₄ spinel ceramics were processed from sub-micrometric commercial powder by applying a two-step procedure: pressureless sintering under vacuum followed by hot isostatic pressing. To limit grain growth and to avoid secondary reactions or impurities, no additives or sintering aids were added to the powder. First, pressureless sintering at 1500 °C during 2 h under vacuum led to opaque samples due to a high level of porosity. To improve the optical quality of the MgAl₂O₄ ceramics and the in-line transmission in the visible range, a post-treatment by hot isostatic pressing was applied. Highly transparent ceramics were obtained after a post-treatment at 1800 °C for 10 h with an in-line transmission of 81% at 400 nm and 86% from 950 to 3000 nm for a thickness of 2 mm (98.8% of the theoretical transmission).     

Dispersion of nano-sized yttria powder using triammonium citrate dispersant for the fabrication of transparent ceramics

In the present work, transparent Y₂O₃ ceramics were prepared via colloidal processing method from nano-sized Y₂O₃ powders. The effects of triammonium citrate (TAC) on the colloid stability of aqueous suspensions of nano-sized Y₂O₃ powders were studied. The surface properties of yttria powders were notably affected by the addition of TAC dispersant. The adsorption of TAC on the particle surface shifts the IEP to lower pH values and increases the absolute zeta potential in alkaline region. Rheological characterization of the investigated system revealed an optimal dispersant concentration of 1 wt%, which correlated well with the saturation adsorption of TAC on Y₂O₃ powder surfaces. The suspensions with solid loadings up to 35 vol% were achieved with further addition of Tetramethylammonium hydroxide (TMAH) into the dispersing system. The consolidated green bodies were treated by cold isostatic pressing to further increase the green density. Transparent Y₂O₃ ceramics were prepared after vacuum-sintering at 1700 °C for 5 h. The transmittances of the sample were 74.5% at 800 nm and 79.8% at 2000 nm, respectively.     

Fabrication of transparent crystal-oriented polycrystalline strontium barium niobate ceramics for electro-optical application

The transparent polycrystalline ceramics with anisotropic crystal system was successfully fabricated by colloidal processing in a high magnetic field and subsequent vacuum sintering and hot isostatic pressing sintering. In this study, we report the fabrication of the transparent c-axis-oriented Sr_0.6Ba_0.4Nb₂O₆ (SBN60) ceramics. The degree of orientation of SBN60 expressed as the Lotgering factor was ∼1.0 and its relative density was over 99.9%. The transmittance of the crystal-oriented SBN60 was 50% at 1500 nm. Optical phase modulation of SBN60 was successfully observed through the measurement of its phase modulation, which confirms the presence of an electro-optical effect.     

Translucent yttrium oxide ceramics from low-density green bodies shaped by uniaxial pressing

Highly compact green bodies are usually required to fabricate transparent or translucent polycrystalline yttrium oxide. The present work reports on the fabrication of highly dense (ρ_rel >98%) translucent Y₂O₃ from low-density green bodies by exploiting a high sinterability of nano Y₂O₃ powder. A commercial nano Y₂O₃, with a crystallite size of ca. 30 nm, was shaped by uniaxial pressing and, afterwards, densified by pre-sintering at 1500 °C followed by hot isostatic pressing. The coarsening tendency of yttria nanoparticles causes the rearrangement of particles and results in the high sinterability of nano Y₂O₃ even at low green densities. This improves the packing density and enables sintering to high densities, eliminating pores, and, thus, obtaining translucent Y₂O₃.     

Infrared‐Transparent Y2O3–MgO Nanocomposites Fabricated by the Glucose Sol–Gel Combustion and Hot‐Pressing Technique

A glucose sol–gel combustion method has been developed to synthesize composite nanopowders with equal volume fractions of Y₂O₃ and MgO. The synthesis involves the generation of precursor foam containing Y³⁺ and Mg²⁺ cations via the chemical and thermal degradation of glucose molecules in aqueous solutions. Subsequent calcination of the foam gave the composite nanopowders uniform composition and surface areas of 44–62 m²/g depending on the relative amount of glucose. Then the nanopowder with an average particle size of 19 nm was consolidated by the hot‐pressing technique with different sintering temperatures. The fabricated nanocomposite is mid‐infrared transparent as the result of fine grains, narrow grain size distribution, and uniform phase domains. The transmittance increases with increase in the sintering temperature and reaches 83.5% at 3–5 μm mid‐infrared wave range once the temperature reaches 1350°C, which is close to the theoretical value of 85%. And it is noteworthy that the cutoff wavelength reaches 9.6 μm, which is superior to those of spinel, AlON, and sapphire. And the Vickers hardness of the sample reaches 10.0 ± 0.1 GPa, which is significantly higher than those of the coarse grained single‐phase MgO and Y₂O₃. The results indicate that the glucose sol–gel combustion and hot‐pressing technique is an effective method to fabricate infrared transparent Y₂O₃–MgO nanocomposites.