Structural and Thermo‐Mechanical Properties of Nd: Y2O3 Transparent Ceramics

Various content of neodymia Nd: Y₂O₃ (Nd: 0.5–5.0 at.%) transparent ceramics were fabricated by vacuum sintering. The prepared Nd: Y₂O₃ ceramics exhibit high transmittance (~80%) at the wavelength of 1100 nm. It is found that the increase in Nd concentration enhances the grain size growth, while decreases the phonon energy, which is benefit for improving both the luminescence quantum and up‐conversion efficiency. The thermal conductivity and thermal expansion coefficient of the transparent 1.0 at.% Nd: Y₂O₃ ceramic is 5.51 W·(m·K)^?1 and 8.11 × 10^?6 K^?1, respectively. The hardness and the fracture toughness of the transparent ceramic is 9.18 GPa and 1.03 Mpa·m^1/2, respectively. The results indicate that the Nd: Y₂O₃ transparent ceramic is a potential candidate material for laser.     

Highly transparent Yb:Y2O3 ceramics obtained by solid-state reaction and combined sintering procedures

(Y_0.87-xLa_0.1Zr_0.03Yb_x)₂O₃ (x?=?0.02, 0.04, 0.05) transparent ceramics were obtained by solid-state reaction and combined sintering procedures with La₂O₃ and ZrO₂ as sintering additives. A method based on two-step intermediate sintering in air followed by vacuum sintering was applied in order to control the densification and grain growth of the samples during the final sintering process. The results indicate that La₂O₃ and ZrO₂ co-additives can improve the microstructure and optical properties of Yb:Y₂O₃ ceramics at relatively low sintering temperature. On the other hand, the addition of Zr⁴⁺ ions leads to the formation of dispersed scattering volumes in the ceramic bodies. Transmittance of 78.8% was measured for the 2.0?at% Yb:Y₂O₃ ceramic sample at the wavelength of 1100?nm. The spectroscopic properties of Yb:Y₂O₃ ceramics were investigated at room temperature. The obtained results show that the absorption cross-section at 978?nm is in the range of 2.08?×?10^–20 to 2.36?×?10^–20 cm², whereas the emission cross-section at 1032?nm is ~1.0?×?10^–20 cm².     

Effects of ZrO2-La2O3 co-addition on the microstructural and optical properties of transparent Y2O3 ceramics

Commercial Y₂O₃ powder was used to fabricate Y₂O₃ ceramics sintered at 1600 °C and 1800 °C with concurrent addition of ZrO₂ and La₂O₃ as sintering aids. One group with different contents of La₂O₃ (0–10 mol%) with a fixed amount of 1 mol% ZrO₂ and another group with various contents of ZrO₂ (0–7 mol%) with a fixed amount of 10 mol% La₂O₃ were compared to investigate the effects of co-doping on the microstructural and optical properties of Y₂O₃ ceramics. At low sintering temperature of 1600 °C, the sample single doped with 10 mol% La₂O₃ exhibits much denser microstructure with a few small intragranular pores while the samples with ZrO₂ and La₂O₃ co-doping features a lot of large intergranular pores leading to lower density. When the sintering temperature increases to 1800 °C, samples using composite sintering aids exhibit finer microstructures and better optical properties than those of both ZrO₂ and La₂O₃ single-doped samples. It was proved that the grain growth suppression caused by ZrO₂ overwhelms the acceleration by La₂O₃. Meanwhile, 1 mol% ZrO₂ acts as a very important inflection point with regard to the influence of additive concentration on the transmittance, pore structure and grain size. The highest in-line transmittance of Y₂O₃ ceramic (1.2 mm in thickness) with 3 mol% of ZrO₂ and 10 mol% of La₂O₃ sintered at 1800 °C for 16 h is 81.9% at a wavelength of 1100 nm, with an average grain size of 11.2 µm.     

Structural and optical properties of Tm:Y2O3 transparent ceramic with La2O3, ZrO2 as composite sintering aid

The paper reports the use of La₂O₃ and ZrO₂ co-doping as a composite sintering aid for the fabrication of Tm:Y₂O₃ transparent ceramics. Two groups of experiments were conducted for investigating the influences of composite sintering aids on the microstructures and the optical properties of Tm:Y₂O₃ transparent ceramics in contrast to single La³⁺ and single Zr⁴⁺ doped Tm:Y₂O₃. Samples with composite sintering aids could realize fine microstructures and good optical properties at relatively low sintering temperatures. Grain sizes around 10 μm and transmittances close to theoretical value at wavelength of 2 μm were achieved for the 9 at.% La³⁺, 3 at.% Zr⁴⁺ co-doped samples sintered at 1500-1600 °C. The influences of the composite sintering aids on the emission intensities and the phonon energies of Tm:Y₂O₃ ceramics were also investigated.     

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.     

Fabrication and properties of macro-porous SiC using Al2O3–Y2O3–SiO2 as bonding additives

Macro-porous SiC was fabricated without using pore-forming agents by an in situ reaction bonding process. A bonding additive, Al₂O₃–Y₂O₃–SiO₂, with a low melting temperature was mixed with SiC particles and sintered at 1500 °C and 1600 °C for 1 h in Ar. Macro-porous SiC with a porosity of 32.7–45.9%, a pore size of 3.4–4.2 μm, and a relatively narrow and uniform pore size distribution was fabricated by varying the amount of bonding additive. The flexural strength of macro-porous SiC prepared at 1500 °C increased from 47.2 MPa to 71.2 MPa while the porosity decreased from 45.9% to 42.8%, respectively. When the sintering temperature of the macro-porous SiC was increased to 1600 °C, the flexural strengths were significantly reduced to 32.6–35.6 MPa, along with a reduction in porosity and pore size. The permeability of macro-porous SiC prepared at 1500 °C varied from 1.59 × 10^?12 m² to 1.26 × 10^?12 m², depending on the porosity. As the sintering temperature increased from 1500 °C to 1600 °C, the permeability decreased to less than 1.00 × 10^?12 m² because of the reduced porosity and average pore size. The electrical resistivity of macro-porous SiC prepared at 1500 °C and 1600 °C varied from 2.7 × 10⁸ Ω-cm to 1.4 × 10⁹ Ω-cm and from 1.3 × 10⁸ Ω-cm to 1.7 × 10⁹ Ω-cm, respectively, with increasing volume percent of bonding additives. The relatively high electrical resistivity was apparently due to neck bonding phase between SiC particles formed by phases consisting of Y₂Si₂O₇, YAG, and residual Al₂O₃.     

Fabrication and properties of pressure-sintered reaction-bonded Si3N4 ceramics with addition of Eu2O3–MgO–Y2O3

Dense pressure-sintered reaction-bonded Si₃N₄ (PSRBSN) ceramics were obtained by a hot-press sintering method. Precursor Si powders were prepared with Eu₂O₃–MgO–Y₂O₃ sintering additive. The addition of Eu₂O₃–MgO–Y₂O₃ was shown to promote full nitridation of the Si powder. The nitrided Si₃N₄ particles had an equiaxial morphology, without whisker formation, after the Si powders doped with Eu₂O₃–MgO–Y₂O₃ were nitrided at 1400 °C for 2 h. After hot pressing, the relative density, Vickers hardness, flexural strength, and fracture toughness of the PSRBSN ceramics, with 5 wt% Eu₂O₃ doping, were 98.3 ± 0.2%, 17.8 ± 0.8 GPa, 697.0 ± 67.0 MPa, and 7.3 ± 0.3 MPa m^1/2, respectively. The thermal conductivity was 73.6 ± 0.2 W m^?1 K^?1, significantly higher than the counterpart without Eu₂O₃ doping, or with ZrO₂ doping by conventional methods.     

Preparation and application evaluation of La2O3-doped Y2O3 crucible materials for melting TiAl alloys

A new La₂O₃-doped Y₂O₃ crucible materials was fabricated and evaluated by TiAl alloys melting test. Microstructure and properties of the La₂O₃-doped Y₂O₃ ceramics were systemically investigated. In addition, interfacial reaction mechanism of the La₂O₃-doped Y₂O₃ crucible materials and TiAl alloys, together with oxygen content of TiAl alloys were discussed. Solid solution of La³⁺ in the crystal lattice of Y₂O₃ significantly improved sintering properties of the La₂O₃-doped Y₂O₃ crucible materials and decreased the open porosity. Compared with pure Y₂O₃, when adding 15 wt% La₂O₃, the open porosity and strength retention ration after thermal shock test of the La₂O₃-doped Y₂O₃ crucible materials changed from 10.8% to 3.9% and from 64% to 78%, respectively. The interfacial reaction between La₂O₃-doped Y₂O₃ crucible materials and TiAl alloys belongs to physical dissolution, and no reaction products were found during the melting of TiAl alloys. When using the 15 wt% La₂O₃-doped Y₂O₃ crucible materials to melt TiAl alloys, oxygen content of the TiAl ingot declined to 530 ppm, which was only one fourth of that using pure Y₂O₃ materials.     

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.     

Synthesis of Ga-doped Li7La3Zr2O12 solid electrolyte with high Li+ ion conductivity

Garnet-type Li₇La₃Zr₂O₁₂ (LLZO) Li⁺ ion solid electrolyte is a promising candidate for next generation high-safety solid-state batteries. Ga-doped LLZO exhibits excellent Li⁺ ion conductivity, higher than 1 × 10^?3 S cm^?1. In this research, the doping amount of Ga, the calcination temperature of Ga-LLZO primary powders, the sintering conditions and the evolution of grains are explored to demonstrate the optimum parameters to obtain a highly conductive ceramics reproducibly via conventional solid-state reaction methods under ambient air sintering atmosphere. Cubic LLZO phase is obtained for Li_6.4Ga_0.2La₃Zr₂O₁₂ powder calcined at low temperature 850 °C. In addition, ceramic pellets sintered at 1100 °C for 320 min using this powder have relative densities higher than 94% and conductivities higher than 1.2 × 10^?3 S cm^?1 at 25 °C.     

Novel amorphous precursor densification to transparent Nd:Y2O3 Ceramics

A novel approach of neodymium ion doped yttrium oxide (Nd:Y₂O₃) amorphous precursor compaction and sintering is being reported for the first time. Precursor of 2 at.% Nd³⁺ doped Y₂O₃ was synthesized by gelation of sol of yttrium and neodymium nitrates with l-alanine at 80 °C for 16 h followed by gel combustion in microwave. A part of microwave precursor was heat treated at 700 °C for 5 h to give the partially crystalline Nd:Y₂O₃ amorphous precursor. Thermogravimetric analysis (TGA) of partially crystalline amorphous precursor of Nd:Y₂O₃ gave 8.5% total weight loss indicating removal of maximum organics. X-Ray diffraction (XRD) showed broad peaks indicating incomplete crystallization of cubic Nd:Y₂O₃. Morphology was found to be close to spherical with particles in size range 17–19 nm by TEM. Another part of microwave precursor on calcination at 1000 °C for 3 h led to formation of fully crystalline Nd:Y₂O₃ with particles in size range of 35–85 nm. Both partially crystalline amorphous precursor and fully crystalline Nd:Y₂O₃ were compacted at 400 MPa by cold isostatic press and sintered at 1750 °C for 10 h under vacuum (10^?5 mbar). The partially crystalline Nd:Y₂O₃ amorphous precursor densified to 99% with 65% transmission at 2500 nm (0.5 mm thickness) compared to 96% densification with 34% transmission for fully crystalline Nd:Y₂O₃ without any sintering aids. Retention of cubic phase purity of Y₂O₃ was observed in both the ceramic pellets post sintering by XRD. Good grain fusion with grain growth to ≤2 μm was observed by scanning electron microscope (SEM) for partially crystalline Nd:Y₂O₃ amorphous precursor. Thus partially crystalline Nd:Y₂O₃ amorphous precursor nanopowders, with homogeneous close to spherical fine particles and high reactivity due to ionic mobility of amorphous phase, led to better densification.     

Phase formation and lattice distortion of Lu2O3-doped ZrO2 in comparison with Y2O3-doped ZrO2

Lu₂O₃ and Y₂O₃ doping of 8, 11, and 18 mol% in ZrO₂ were prepared by solid solution reaction, aiming to study the phase stabilization of Lu₂O₃-doped ZrO₂ and Y₂O₃-doped ZrO₂ in terms of phase formation and lattice distortion. The Rietveld refinement results indicated that Lu₂O₃-doped ZrO₂ and Y₂O₃-doped ZrO₂ followed the same trend in terms of cubic phase fraction, increasing from 25%–30% (8 mol%) to 95%–100% (11 and 18 mol%). This phase formation was confirmed by observing the same diffraction ring pattern observed for the Lu₂O₃-doped ZrO₂ and Y₂O₃-doped ZrO₂. The Vickers hardness of the Lu₂O₃-doped ZrO₂ was 4.3% higher than that of Y₂O₃-doped ZrO₂ at 8 mol%, but 9.7% and 14.8% lower at 11 and 18 mol%, respectively. This was likely caused by the lattice distortion effect of Y₂O₃ doping overpowering the field strength difference between Lu³⁺ and Y³⁺.     

Preparation of transparent Y2O3 ceramic via gel casting: Realization of high solid volume via surface modification

In this article, isocyanate was adopted to modify Y₂O₃ powder for the purpose of preparing transparent Y₂O₃ ceramics via gel casting. The modification could enhance the hydration resistance of Y₂O₃ powder through the steric hindrance effect. The coating mechanism can be proved by the infrared spectrum of the surface-modified Y₂O₃ powder. Modification could not only prevent Y₂O₃ particles from reacting with water, but also prevents agglomeration between particles. The viscosity of the slurry with a solid content of 52.7 vol% is only 0.48 Pa·s at the shear rate of 100 s⁻¹, which is suitable for preparing high-density compacts by gel casting. The transmittance of the sample (1840°C × 8 h, 1 mm thickness) at 1100 nm reaches 75%. The microstructure of the sintered body is dense with the average grain size of 6.5 μm without obvious impurities nor pores. Five mol% ZrO₂-doped Y₂O₃ transparent ceramic fairing with the diameter of 5 cm without defects was successfully fabricated by gel casting (52.7 vol% solid volume) and vacuum sintering (1840°C × 8 h).     

Electrical characterization of La9.33Si2Ge4O26 oxyapatite for prospective intermediate-temperature solid oxide fuel cells

La_9.33Si₂Ge₄O₂₆ materials have been fabricated from La₂O₃, SiO₂ and GeO₂ powders by high speed mechanical alloying followed by conventional and microwave hybrid sintering at different temperatures and holding times. XRD data showed that the apatite phase is formed after 1 h of mechanical alloying at 850 rpm. This phase remained stable after conventional sintering in an electric furnace with density increasing as sintering temperatures and holding times were increased. However, the highest density was achieved for samples sintered in the microwave furnace (5.44 g cm⁻³), corresponding to a relative density of 98%. The electrical conductivity of the samples microwave sintered at 700 and 800 ºC are 4.72×10⁻³ and 1.93×10⁻² S.cm⁻¹, respectively, with a correspondent activation energy of 0.952 eV.     

Sintering,microstructure and mechanical properties of Al2O3–Y2O3–ZrO2 (AYZ) eutectic composition ceramic microcomposites

We report on how the mechanical properties of sintered ceramics (i.e., a random mixture of equiaxed grains) with the Al₂O₃–Y₂O₃–ZrO₂ eutectic composition compare with those of rapidly or directionally solidified Al₂O₃–Y₂O₃–ZrO₂ eutectic melts. Ceramic microcomposites with the Al₂O₃–Y₂O₃–ZrO₂ eutectic composition were fabricated by sintering in air at 1400–1500 °C, or hot pressing at 1300–1400 °C. Fully dense, three phase composites of Al₂O₃, Y₂O₃-stabilized ZrO₂ and YAG with grain sizes ranging from 0.4 to 0.8 μm were obtained. The grain size of the three phases was controlled by the size of the initial powders. Annealing at 1500 °C for 96 h resulted in grain sizes of 0.5–1.8 μm. The finest scale microcomposite had a maximum hardness of 19 GPa and a four-point bend strength of 282 MPa. The fracture toughness, as determined by Vickers indentation and indented four-point bending methods, ranged from 2.3 to 4.7 MPa m^1/2. Although strengths and fracture toughnesses are lower than some directionally or rapidly solidified eutectic composites, the intergranular fracture patterns in the sintered ceramic suggest that ceramic microcomposites have the potential to be tailored to yield stronger, tougher composites that may be comparable with melt solidified eutectic composites.     

Phase stability and mechanical properties of TZP with a low mixed Nd2O3/Y2O3 stabiliser content

The phase assembly of 1.0–5.0 mol% Nd₂O₃-doped ZrO₂ sintered at 1400 °C revealed that the tetragonal ZrO₂ phase could not be completely stabilised. Co-stabilising of 0.5–2.5 mol% Nd₂O₃ with 0.5–1.0 mol% Y₂O₃, however, allowed the preparation of fully dense (Nd,Y)-TZP ceramics by pressureless sintering in air at 1450 °C. The mixed stabiliser monoclinic zirconia nanopowder starting material was synthesized from a suspension of neodymium nitrate, yttrium nitrate and monoclinic zirconia powder in an alcohol/water mixture. A HV₃₀ hardness of 10 GPa combined with an excellent indentation toughness of 13 MPa m^1/2 could be achieved for the (1.0Nd,1.0Y)- and (1.5Nd,1.0Y)-TZP ceramics. The influence of the mixed stabiliser content on the phase stability and mechanical properties are investigated and discussed.     

High oxide ion conduction in sintered oxides of the system Bi2O3-Y2O3

The ionic conduction in sintered Bi₂O₂-Y₂O₃ was investigated by measuring the conductivity and the emf of an oxygen concentration cell using the specimen tablet as electrolyte. The face centred cubic phase in this system was found to show high oxide ion conduction accompanied by a little electronic conduction when exposed to air. This phase was stable with a composition of 25 ～ 43 mol % Y₂O₃ over a wide range of temperatures, and the oxide ion conductivity increased with decrease in Y₂O₃. The conductivities of (Bi₂O₃)_0.75 (Y₂O₃)_0.25 were 1.6×10^?1 Ω^?1 cm^?1 at 700°C and 1.2×10^?2 Ω^?1 cm^?1 at 500°C values which are many times higher than those of stabilized zirconia (ZrO₂)_0.90(Y₂O₃)_0.10 at corresponding temperatures. Specimens containing less than 25 mol % Y₂O₃ showed a phase transition at 700 ～ 580°C and the conductivities decreased remarkably below these temperatures. High oxide ion conduction in the fcc phase is attributed to the migration of oxide ion vacancies which were present in an appreciable amount.     

Microstructure and mechanical properties of Al2O3/Y3Al5O12/ZrO2 hypereutectic directionally solidified ceramic prepared by laser floating zone

Al₂O₃/Y₃Al₅O₁₂/ZrO₂ directionally solidified ceramic has been considered as a promising candidate for ultrahigh temperature structural materials due to its excellent performance even close to its melting point. In this work, laser floating zone (LFZ) solidification experiments were performed on Al₂O₃/Y₃Al₅O₁₂/ZrO₂ hypereutectic with the solidification rates between 2 μm/s and 30 μm/s. The full eutectic lamellar microstructure is obtained with hypereutectic composition. The solid/liquid interface morphology is investigated. The microstructure characteristic is discussed based on the solid/liquid interface. The variation of lamellar spacing with different compositions and solidification rates was reported and discussed by considering an irregular eutectic growth model. The maximum hardness and fracture toughness are 19.06 GPa and 3.8 MPa m^1/2, respectively. The toughening mechanism of ZrO₂ is discussed based on the scenario of the crack propagation pattern.     

The absorption and emission properties of highly transparent ZrO2-doped Yb3+: Y2O3 ceramics

Ultra-highly transparent ZrO₂-doped Yb³⁺: Y₂O₃ ceramics were prepared by slip casting and vacuum pressureless sintering and the transmittance reached the highest value of 80.9% for the sample doped with 8.0 at% Yb³⁺. There are three main absorption peaks at 905, 950, and 976 nm, corresponding to the transition from the lowest level of field splitting of ²F_7/2 crystal to every splitting energy levels of ²F_5/2 crystal field. We analyzed the absorption and emission spectra of transparent Yb³⁺: Y₂O₃ from the energy level structure of Yb³⁺, and the transmission, absorption, and emission spectra were systematically studied. There are three main absorption peaks at 905, 950, and 976 nm and four emission peaks at 1076, 1031, 1013, and 977 nm, respectively. The emission peaks at 977 and 1013 nm broaden and vanish for 8.0 and 10.0 at% Yb³⁺-doped Y₂O₃, which may be related to the change of Y₂O₃ crystal field caused by high concentration.     

Effects of Al2O3–Y2O3/Yb2O3 additives on microstructures and mechanical properties of silicon nitride ceramics prepared by hot-pressing sintering

Silicon nitride (Si₃N₄) ceramics doped with two different sintering additive systems (Al₂O₃–Y₂O₃ and Al₂O₃–Yb₂O₃) were prepared by hot-pressing sintering at 1800℃ for 2 h and 30 MPa. The microstructures, nano-indentation test, and mechanical properties of the as-prepared Si₃N₄ ceramics were systematically investigated. The X-ray diffraction analyses of the as-prepared Si₃N₄ ceramics doped with the two sintering additives showed a large number of phase transformations of α-Si₃N₄ to β-Si₃N₄. Grain size distributions and aspect ratios as well as their effects on mechanical properties are presented in this study. The specimen doped with the Al₂O₃–Yb₂O₃ sintering additive has a larger aspect ratio and higher fracture toughness, while the Vickers hardness is relatively lower. It can be seen from the nano-indentation tests that the stronger the elastic deformation ability of the specimens, the higher the fracture toughness. At the same time, the mechanical properties are greatly enhanced by specific interlocking microstructures formed by the high aspect ratio β-Si₃N₄ grains. In addition, the density, relative density, and flexural strength of the as-prepared Si₃N₄ ceramics doped with Al₂O₃–Y₂O₃ were 3.25 g/cm³, 99.9%, and 1053 ± 53 MPa, respectively. When Al₂O₃–Yb₂O₃ additives were introduced, the above properties reached 3.33 g/cm³, 99.9%, and 1150 ± 106 MPa, respectively. It reveals that microstructure control and mechanical property optimization for Si₃N₄ ceramics are feasible by tailoring sintering additives.