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.     

Synthesis of highly-infrared transparent Y2O3–MgO nanocomposites by colloidal technique and SPS

Infrared (IR) transparent Y₂O₃–MgO nanocomposites with a volume ratio of 50:50 were synthesized by combining colloidal and spark-plasma-sintering (SPS) techniques. In order to attain well-dispersed and homogeneous starting Y₂O₃–MgO nanopowder mixture, the effects of the pH value and the amount of polyetherimide (PEI) dispersant on the suspension stability were studied. Rheological measurement reveals that highly-dispersed and stable suspension was obtained at 7 wt% of PEI dispersant under pH = 10.6. The obtained nanopowders with particle size of 20–30 nm were densified using SPS at several sintering temperatures. The sintered composites show fine grains, narrow grain size distribution and uniform microstructure. The nanocomposite sintered at 1250 °C showed the maximum IR transmittance of 84% at a wavelength range of 2.5–6 μm. The Vickers hardness of the nanocomposite was about 11.9 ± 0.3 GPa, which is significantly higher than those of single phase MgO or Y₂O₃. Successful fabrication of the high-performance Y₂O₃–MgO nanocomposite indicates that i) the colloidal technique is an effect method to obtain highly dispersed and homogeneous nanopowders and ii) the SPS technique is a powerful tool to fabricate fine-grained dense transparent ceramics, which are suitable for fabricating IR transparent Y₂O₃–MgO composite ceramics from commercial starting powders.     

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.     

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.     

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.     

Rapidly fabricating Y2O3 transparent ceramics at low temperature by SPS with mesoporous powder

Fine-grained and dense highly transparent Y₂O₃ ceramics have been successfully prepared using high sintering activity mesoporous Y₂O₃ powders without any additive by spark plasma sintering (SPS). The influences of the sintering temperature on microstructure, density, optical, and mechanical properties of SPS-sintered Y₂O₃ ceramics were studied in detail. As results, the optimal Y₂O₃ ceramics with high relative density of 99.90% and fine average grain size of 140 nm were obtained at a low sintering temperature of 1140°C and a moderate load pressure of 60 MPa for 5 min. Meanwhile, the dense Y₂O₃ ceramics with 1 mm thickness after annealing show a high linear transmittance of 78% (close to 94% of the theoretical value) at 2.4–3 µm wavelength. In additions, the Vickers hardness and fracture toughness of samples can reach 8.48 GPa and 1.45 MPa m^1/2, respectively. This result proves that the high activity of mesoporous Y₂O₃ is considered to be an important means for preparing high-performance fine Y₂O₃ ceramics at low sintering temperature.     

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.     

Gel-casting of MgAl2O4 transparent ceramics using a common dispersant

The ethanolaminic salt of citric acid (commercial name Dolapix CE 64) has commonly been used as a dispersant for colloidal based ceramic forming process. In this paper, a surprise was presented that MgAl₂O₄ spinel slurries consisting of MgAl₂O₄ spinel nanoparticles and Dolapix CE 64 gelled in air at room temperature spontaneously. The MgAl₂O₄ spinel slurries with high solid loading (54 vol%) were prepared with Dolapix CE 64 and the green body with up to 57% relative density was obtained. MgAl₂O₄ transparent ceramics with small grain size (0.92 μm) and high transmittance (81.7% at 600 nm) were fabricated after pre-sintering at 1500°C and hot-isostatic sintering at 1550°C.     

Effect of milling ball size on the densification and optical properties of transparent Y2O3 ceramics

In this study, we report highly transparent Y₂O₃ ceramics fabricated by hot-pressing only at 1500 °C without a HIP treatment, featuring in-line transmittance levels of 77% and 84% at a wavelength of 400 and 1100 nm, respectively with the grain size suppressed to 710 nm. The effect of the ball size during the grinding of Y₂O₃ powders on the correlation between the thus-prepared Y₂O₃ powders and the optical properties of the hot-pressed samples is demonstrated for the first time. With a decrease in the diameter of the ZrO₂ balls from 5 mm to 1 mm, the milling efficiency was enhanced and admirable transparency of Y₂O₃ was attained at a short milling time. However, several micron-sized pores remained in the transparent specimens prepared with 1 mm balls, originating from the inhomogeneously packed region of the green body. Finally, the 2 mm was found to be optimum for obtaining a fine-grained and pore-free microstructure with the best in-line transmittance of Y₂O₃ ceramics.     

Effects of pre-sintering and annealing on the optical transmittance of Zr-doped Y2O3 transparent ceramics fabricated by vacuum sintering conjugated with post-hot-isostatic pressing

In this work, Zr-doped Y₂O₃ transparent ceramics were fabricated by vacuum pre-sintering at various temperatures ranging from 1650 to 1800 °C combined with a post-hot-isostatic pressing (HIP) treatment. The pre-sintered samples all show black opaqueness mainly due to the formation of oxygen vacancies, which can be removed by post-annealing in air. The HIP treatment can also eliminate the blackness as well as residual pores, giving rise to optical transparency. The in-line transmittance of the samples after HIP was found to depend strongly on the microstructure of the as-sintered samples. The optimal microstructure of these types of samples before the HIP treatment should be fine grained with only intergranular pores, which can easily be removed by HIP. Annealing before HIP was shown to be necessary to enhance the transmittance of the samples. The effects of the pre-sintering heating rate on the optical transmittance of the HIP-treated samples were also studied.     

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.     

Effect of La2O3 on the microstructure and optical performance of (Tb0.8Y0.2-xLax)2O3 ceramics

(Tb_0.8Y_0.2-xLa_x)₂O₃ transparent ceramics were prepared by using co-precipitation method combined with pressure-less sintering in flowing H₂ atmosphere. Microstructure, optical transmittance, elements composition, and Verdet constant of the (Tb_0.8Y_0.2-xLa_x)₂O₃ ceramics were studied. The amount of La₂O₃ is crucial for the formation of expected transparent (Tb_0.8Y_0.2)₂O₃. With increasing content of La₂O₃, the number of pores and the grain size of as-fabricated (Tb_0.8Y_0.2-xLa_x)₂O₃ ceramics both decrease. When 4 at.% La₂O₃ is doped, the (Tb_0.8Y_0.16)₂O₃ transparent ceramics shows the highest transmittance of 73.3% at 1400 nm wavelength. With holding time increasing from 8 h to 15 h, the average grain size of (Tb_0.8Y_0.16La_0.04)₂O₃ ceramics gradually increases from 5 μm to 13 μm. The Verdet constant measured at 633 nm is ?352 rad/T·m, which is 2.63 times higher than that of TGG. In addition, large-size ceramics with Φ 20 mm × 3 mm and Φ 30 mm × 3 mm were also successfully obtained.     

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.     

Fabrication and characterization of highly transparent Er:Y2O3 ceramics with ZrO2 and La2O3 additives

In this study, we report highly transparent Er:Y₂O₃ ceramics (0–10 at% Er) fabricated by a vacuum sintering method using compound sintering additives of ZrO₂ and La₂O₃. The transmittance, microstructure, thermal conductivity and mechanical properties of the Er:Y₂O₃ ceramics were evaluated. The in-line transmittance of all of the Er:Y₂O₃ ceramics (1.2 mm thick) exceeds 83% at 1100 nm and 81% at 600 nm. With an increase in the Er doping concentration from 0 to 10 at%, the average grain size, microhardness and fracture toughness remain nearly unchanged, while the thermal conductivity decreases slightly from 5.55 to 4.89 W/m K. A nearly homogeneous doping level of the laser activator Er up to 10 at% in macro-and nanoscale was measured along the radial direction from the center to the edge of a disk specimen, which is the prominent advantage of polycrystalline over single-crystal materials. Based on the finding of excellent optical and mechanical properties, the compound sintering additives of ZrO₂ and La₂O₃ are demonstrated to be effective for the fabrication of transparent Y₂O₃ ceramics. These results may provide a guideline for the application of transparent Er:Y₂O₃ laser ceramics.     

Study on the effect and mechanism of zirconia on the sinterability of yttria transparent ceramic

Transparent Y₂O₃ ceramics were fabricated by solid-state reaction using high purity Y₂O₃ and ZrO₂ powder as starting material. The results indicated that ZrO₂ additive can improve the transparency of Y₂O₃ ceramic greatly. The best transmittance appears with 3 at.% ZrO₂ doped Y₂O₃ transparent ceramic with transmittance at 1100 nm of 83.1%, which is up to 98.6% of the theoretical value. The microstructure is uniform and no secondary phase is observed in the ceramic with the average grain size of 15 μm. The mechanism of ZrO₂ improving the transparency of Y₂O₃ ceramic is analyzed in detail. On this basis, Yb³⁺ doped Y₂O₃ transparent ceramic was also fabricated and spectroscopic properties were investigated.     

ZrO2-doped Y2O3 transparent ceramics via slip casting and vacuum sintering

Commercial Y₂O₃ powder was used to fabricate highly transparent Y₂O₃ ceramics with the addition of ZrO₂ via slip casting and vacuum sintering. The effects of ZrO₂ addition on the transparency, grain size and lattice parameter of Y₂O₃ ceramics were studied. With addition of ZrO₂ the transparency of Y₂O₃ ceramics increased markedly and the grain size of Y₂O₃ ceramics decreased markedly by cation diffusivity mechanism and the lattice parameter of Y₂O₃ ceramics slightly decreased. The highest transmittance (at wavelength 1100 nm) of the 5.0 mol% ZrO₂–Y₂O₃ ceramic (1.0 mm thick) sintered at 1860 °C for 8 h reached 81.7%, very close to the theoretical value of Y₂O₃.     

The effect of slip casting parameters on the green density of MgAl2O4 spinel

The aim of this paper was to investigate the effect of slip casting parameters on the green density of MgAl₂O₄ spinel. In order to obtain samples with suitable mechanical and optical properties, it is necessary to prepare bulk samples with a fine grain size along with a low level of impurity and high density. Slip casting is widely used in the processing of optical ceramics to achieve a body with high green density and low sintering temperature. In the present study, several spinel suspensions with similar solid content but different viscosities and particle sizes (90, 150, 300 and 500 nm) were prepared and shaped into a dense body. Viscosity of suspension depended on dispersant content, such that the addition of dispersant firstly caused viscosity to decrease, but it was increased by further dispersant addition, irrespective of the suspension particle size. The green density range of samples was 36–67% of the theoretical value. Rheological behaviour and green density measurements showed that powder particles smaller than 90 nm were unsuitable for slip casting because agglomeration of powder particles led to high viscosity and hence, low green density. The optimal particle size for slip casting was found to be 150 nm.     

Effect of yttria substitution on structure,optical and mechanical properties of (Gd,Y)2O3–MgO nanocomposite ceramics

A citrate-nitrate combustion method was applied to synthesize fine composite Gd_2-xY_xO₃-MgO (x = 0, 0.02, 0.2, 0.3, 0.4, 0.6) nanopowders. Y₂O₃ substitution inhibited Gd₂O₃ phase transition from cubic structure to monoclinic structure during sintering, thereby stabilizing its cubic structure to room temperature. This approach led to nanocomposite ceramics with a grain size of about 190 nm and increased the transmittance to 85% over the 3–5 μm wavelength range when x = 0.3. However, the addition of Y₂O₃ weakened the mechanic properties of the nanocomposite ceramics.     

Formulation and preparation of low-concentrated yttria colloidal dispersions

High-temperature creep resistant steels for nuclear applications consist of a steel matrix reinforced with a dispersion of nano-sized refractory ceramic oxide particles, e.g. yttria (Y₂O₃). In this study, the formulation and preparation of low-loaded (2, 3 and 4 vol.%) Y₂O₃ colloidal dispersions for its possible application as suspension precursor in the production of high-temperature creep resistant steels is discussed. The final end product is formulated as a low-concentrated and low-viscous colloidal suspension consisting of non-agglomerated Y₂O₃ nano-particles in the (sub)-100 nm range.The spherical as-received and submicron agglomerated powder necessitates ball-mill processing in order to reduce the as-received size distribution down to nano-level. A comparative study on the desagglomeration of Y₂O₃ nano-powder using conventional planetary ball-milling or nano-milling technology has been done. Formulation of stable colloidal suspensions by screening suitable dispersants has led to the selection of one specific dispersant for this application, Calgon N. Suspension characterization by the determination of particle size distribution (PSD), ζ-potential measurements, colloidal suspension visualization using transmission electron microscopy (TEM), rheology and suspension life-time is discussed in this paper.     

Coating Y2O3 nano-particles with ZrO2-additive via precipitation method for colloidal processing of highly transparent Y2O3 ceramics

In the present work, transparent Y₂O₃ ceramics were prepared via colloidal processing method using ZrO₂-coated nano-sized Y₂O₃ powders. The chemical precipitation method was adopted for the coating of Y₂O₃ raw powder. The evolution of the coated-ZrO₂ layer upon calcination was studied. The rheological behaviors of the slurries of Y₂O₃ powders coated with different content of ZrO₂-additive were investigated. The pH_IEP of ZrO₂-coated Y₂O₃ powders shows intermediate values between that of raw Y₂O₃ and ZrO₂ powders. As the ZrO₂-coating concentration increased from 0 to 5.0 at%, the magnitude of the negative zeta potential at pH > pH_IEP shows a general trend of increment, whereas it decreased at pH < pH_IEP. The viscosity decreases pronouncedly with the increase of ZrO₂ content from 0.5 at% to 3.0 at%. The suspensions with low viscosity and high stability was achieved for a solid loading of 35.0 vol% using Y₂O₃ powders coated with 5.0 at% ZrO₂. The dispersed suspensions were consolidated by centrifugal casting method and the green bodies shown improved homogeneity. Transparent Y₂O₃ ceramics were fabricated by vacuum sintering at 1800 ℃ for 5 h. Transmittance at wavelength 800 nm (1.0 mm thick) reached 80.8%, close to the theoretical value of Y₂O₃.