Transparent Er2O3 ceramics fabricated by high-pressure spark plasma sintering

Fabrication of transparent Er₂O₃ ceramics was carried out by high-pressure spark plasma sintering (HP-SPS). The color and in-line transmittance of these ceramics was highly sensitive to the sintering parameters. Samples exhibited a strong pink or wine color after sintering at 1150 °C under 600 MPa or 1250 °C under 250 MPa, respectively. This was confirmed to be a result of oxygen vacancies created during the sintering process and high sensitivity of Er₂O₃ to the strong reducing atmosphere in the SPS apparatus. Post-sintering annealing in an air furnace led to elimination of oxygen vacancies and increased transparency. Additionally, the photoluminescence intensity and phosphorescence lifetime of annealed (pink) samples was higher and shorter, respectively, compared to that of the reduced (wine-colored) samples.     

Optical and mechanical properties of transparent alumina fabricated by high-pressure spark plasma sintering

Transparent alumina was fabricated from untreated commercial powder by high-pressure spark plasma sintering (HPSPS) at temperatures of 1000, 1050 and 1100 °C under pressures of 250-800 MPa. It was established that transparency strongly depends on the HPSPS parameters. At all temperatures, there was a certain point when increasing the pressure led to decreasing transparency. At 1100 °C, relatively high pressure led to excessive grain growth, as well as the formation of creep-induced porosity at the center of the samples. Hardness values decreased with pressure due to grain growth, correlated with the Hall-Petch relationship. The optimal combination of optical and mechanical properties (68% in-line transmittance at a wavelength of 640 nm and a hardness value of about 2300 HV2) was achieved after sintering at 1050 °C under 600 MPa.     

Co2+:MgAl2O4 saturable absorber transparent ceramics fabricated by high-pressure spark plasma sintering

Single-stage processing of high-quality transparent functional polycrystalline ceramics is desirable but challenging. In the present work, spark plasma sintering (SPS) was employed for fabrication of Co²⁺:MgAl₂O₄ saturable absorbers for laser passive Q-switching. Densification of commercial MgAl₂O₄ powders, doped via co-precipitation, was carried out by conventional SPS and high-pressure SPS (HPSPS) under pressures of 60 and 400 MPa, respectively. The presence of LiF, a common sintering additive, was detrimental to optical properties as it promoted reaction of cobalt with sulfur impurities and the formation of Co₉S₈ inclusions. Densification by HPSPS without LiF allowed to obtain highly transparent Co²⁺:MgAl₂O₄. The optical properties of samples, with doping concentrations varying between 0.01 and 0.1 at.% Co²⁺, were assessed and saturable absorption was demonstrated at ~1.5 µm wavelength, exhibiting ground-state (σ_gs) and excited (σ_es) cross-sections of 3.5×10^-19 and 0.8×10^-19 cm², respectively. Thus, it was established that HPSPS is an effective method to fabricate transparent Co²⁺:MgAl₂O₄ ceramics.     

Post-annealing effect on transparent Mg-Zn aluminate solid solutions fabricated by spark plasma sintering

In MgAl₂O₄ (Mg aluminate) fabricated by pressure sintering, carbon contamination, oxygen vacancy, and other defects exist and cannot be completely removed even after post-annealing. ZnAl₂O₄ (Zn aluminate) has the same crystallographic structure as Mg aluminate and excellent light transmission by post-annealing. In this study, the transmission of (Mg_1-XZn_X)Al₂O₄ spinel, which is a solid solution between Mg aluminate and Zn aluminate, was investigated. After post-annealing, the transmission of (Mg_1-XZn_X)Al₂O₄ spinel was higher than Zn aluminate and Mg aluminate, which means that the absorption center disappeared. Besides, the real in-line transmission is improved by up to 30% by post-annealing, which is related to the driving force to increase the configurational entropy and form a more stable solid solution phase. In solid solution spinel, as the Zn content increases, the optical properties can be improved by post-annealing, but the mechanical properties are slightly decreased.     

Optical,thermal properties,and hydrolysis resistance of transparent YF3-doped CaO ceramics fabricated by vacuum sintering

Transparent calcium oxide (CaO) ceramic was successfully fabricated by pressureless vacuum sintering technique with 0.5 at% YF₃ as the sintering additive. In consideration of the hydrolysis of CaO, the precursor powders were calcined at 600 °C. Within the sintering temperature range of 1150–1450 °C, the effect of YF₃ additive on the phase structure, relative density, transmittance, and microstructure of CaO ceramics was studied. Benefiting from the assisted liquid-phase sintering mechanism and vacancy diffusion mechanism of YF₃, full-dense (3.35 g/cm³) YF₃-doped CaO transparent ceramic was fabricated at 1350 °C with high thermal conductivity of 15.42 W/(m·K). The in-line transmittance attained 47.10% at the wavelength of 1200 nm. Moreover, the hydrolysis resistance was extremely enhanced due to the pore-free structure. Compared to the CaO ceramic with low relative density of 78.66%, the weight gain of full-dense CaO ceramic greatly decreased from 22% to 1.2% within 35 days.     

Fabrication of Lu2Ti2O7-Lu3NbO7 solid solution transparent ceramics by spark plasma sintering and their electrical conductivities

The Lu₂Ti₂O₇-Lu₃NbO₇ system, belonging to A₂B₂O₇ with a cubic structure, is attractive for tailored properties by substitution. In this study, Lu_2+0.25xTi_2−0.5xNb_0.25xO₇ (x = 0–4) transparent ceramics were fabrication by reactive spark plasma sintering using commercially available Lu₂O₃, TiO₂ and Nb₂O₅ powders. The phase evolution, microstructure, density, transmittance and electrical conductivity were investigated as a function of composition parameter x. The results showed that Lu_2+0.25xTi_2−0.5xNb_0.25xO₇ transparent ceramic had a pyrochlore structure at x = 0 and 1, while preserved a defect-fluorite structure at x = 2–4. The lattice parameter and theoretical density increased linearly, while the average grain size decreased steadily with increasing composition parameter x. All the specimens exhibited a dense microstructure and the highest in-line transmittance was 64% at 550 nm for x = 4. The bulk conductivity increased with increasing x, reaching a maximum value of 4.2 × 10⁻² S m^-1 for Lu₃NbO₇ at 1073 K.     

Microstructure and properties of Al2O3-TiC-Ti3SiC2 composites fabricated by spark plasma sintering

Abstract

Abstract

Highly densified Al₂O₃-TiC-Ti₃SiC₂ composites were fabricated by spark plasma sintering technique and subsequently characterised. From fracture surface observation, it is found that Al₂O₃ is 0·2-0·4?μm, TiC is 1-1·5?μm and Ti₃SiC₂ is 1·5-5?μm in grain size. With the increase in Ti₃SiC₂ volume contents, Vickers hardness of the composites decreases because of the low hardness of monolithic Ti₃SiC₂. The fracture toughness rises remarkably when the contents of Ti₃SiC₂ increase, which is attributed to the pullout and microplastic deformation of Ti₃SiC₂ grains. At the same time, the flexural strength of the composites shows a considerable improvement as well. The electrical conductivity rises significantly as the Ti₃SiC₂ contents increase because of the formation of Ti₃SiC₂ network and the increase in conductive phase contents.     

Nano-structured MgAl2O4 spinel consolidated by high pressure spark plasma sintering (HPSPS)

Nano-structured transparent polycrystalline magnesium aluminate spinel (PMAS) was fabricated using a high pressure (up to 1000 MPa) spark plasma sintering (HPSPS) apparatus and various properties of the spinel, such as transparency, micro-structure and mechanical properties (specifically, hardness and fracture toughness), were tested. Using a creep densification model, it was concluded that densification in the final stage of HPSPS is controlled by grain boundary sliding (GBS), rather than by oxygen diffusion. The average grain size of PMAS fabricated under 400 MPa pressure at 1200 °C was about 170 nm, while for samples fabricated under 1000 MPa at 1000 °C the average grain size was remarkably smaller (about 50 nm). HRTEM analysis clearly demonstrated clean grain boundaries and triple points with no evidence for the existence of amorphous regions. Fully dense specimens displayed in-line transmittance higher than 80%. It was moreover established that hardness and fracture toughness values did not depend on the indentation load applied. Finally, hardness values for grains sized between tens of microns and tens of nm strictly followed the Hall-Petch relationship.     

Preparation and properties of novel Tb3Sc2Al3O12 (TSAG) magneto-optical transparent ceramic

Novel Tb₃Sc₂Al₃O₁₂ (TSAG) magneto-optical transparent ceramic was fabricated by vacuum sintering. The phase composition, microstructure, optical quality, thermal properties, and magneto-optical properties of TSAG ceramic were measured. It is shown that the increase in holding time has an effect on the grain size of TSAG ceramic. It is noted that TSAG35 ceramic presents the highest transmittance, corresponding to 81.5 % at the wavelength of 1064 nm. The thermal properties of TSAG ceramic are close to or superior to that of the reported TSAG and TGG crystals. The Verdet constant of TSAG ceramic is comparable to that of reported TSAG crystal, and 1.2 times that of TGG crystal. The results indicate that the novel TSAG ceramic is comparable to TSAG crystal in terms of magneto-optical properties and superior to TGG crystal, making it a candidate material for magneto-optical materials to be used in high-power lasers.     

Spark plasma sintering of transparent Y2O3 ceramic using hydrothermal synthesized nanopowders

Y₂O₃ nanopowders were synthesized by the hydrothermal treatment of Y(NO₃)₃·6H₂O and citric acid (CA) as Y⁺³ and the capping agent, respectively. The effect of different CA:Y⁺³ mol ratios, heat treatment time, and calcination temperature was investigated in order to determine their influence on the morphology, particle size and phase of Y₂O₃ nanopowders. The narrow size distribution of particles was obtained with CA:Y⁺³ mol ratio=1.6, heat treatment time of 6 h, and a calcination temperature at 900 °C for 90 min. Then, the synthesized Y₂O₃ nanopowder was consolidated by the spark plasma sintering technique at 1500 °C with a heating rate of 100 °C/min and held for 8 min before turning off the power. As a result, the ceramic prepared with 3 mm thickness got the highest transmission of 80% at 2.5–6 µm wavelength. The highest density and the grain size of yttria ceramic were 99.58% and 1–1.2 µm at 1500 °C, respectively.     

Optical and thermo-mechanical properties of fine-grained transparent yttria ceramics fabricated by hot-press sintering for infrared window applications

In this work, highly transparent yttria ceramics Φ?=?55?mm in size were fabricated by a hot-pressing method with 1 at.% ZrO₂ or 12 at.% La₂O₃ as a sintering additive. For a 4-mm-thick specimen doped with ZrO₂, the in-line transmittance reaches 71.1% at 400?nm and 80.9% at 1100?nm, and the transmittance of the La₂O₃-doped specimen is comparable to that of the ZrO₂-doped specimen. By means of the relatively low sintering temperature of 1600?°C, the present samples exhibited very fine microstructures (<2?μm), giving rise to excellent mechanical strength levels (～200?MPa). With regard to the 1 at.% ZrO₂-doped specimen, the combination of high strength and high thermal conductivity (～10 W/m?K) substantially improved parameters related to the thermal shock resistance. The results of this study indicate that the hot-pressed transparent yttria ceramic doped with 1 at.% ZrO₂ is optically, mechanically, and thermally suitable for high-temperature IR window applications.     

Vacuum sintering of transparent Cr:Y2O3 ceramics

0–0.7 at% Cr:Y₂O₃ transparent ceramics were prepared by vacuum sintering. The optimum in-line transmittance in the visible and near infrared region is 78%, and the Vickers hardness of the sintered 0.1 at% Cr:Y₂O₃ is 10.1 GPa, respectively. The mechanism of Cr-doped and the optical properties has been discussed. The results indicated that the Cr:Y₂O₃ transparent ceramic is a promising laser material with enhanced mechanical property.     

Polycrystalline transparent magnesium aluminate spinel processed by a combination of spark plasma sintering (SPS) and hot isostatic pressing (HIP)

A two-stage processing approach combining spark plasma sintering (SPS) and hot isostatic pressing (HIP) was employed for the fabrication of relatively large (30?mm diameter) and thick (up to 8?mm) samples of transparent polycrystalline magnesium aluminate. The effects of sample thickness, heating rate during SPS, and the temperature and duration of HIP treatments were investigated. It was established that the heating rate during SPS had a major influence on discoloration due to carbon contamination, which increased with sample thickness. HIP treatment allowed for the elimination of cloudiness due to samples porosity, although carbon contamination present after the SPS step could not be reduced by HIP treatment, regardless of the temperature and duration applied. Highly transparent specimens with thicknesses of 4 and 8?mm exhibiting an in-line transmittance of 85.2 and 83.2% at 600?nm, respectively, were fabricated.     

Gd3Al3Ga2O12:Ce,Mg2+ transparent ceramic phosphors for high-power white LEDs/LDs

Gd₃Al₃Ga₂O₁₂:1.5%Ce, xMg²⁺ (GAGG:1.5%Ce, xMg²⁺) transparent ceramic phosphors (TCPs) were prepared via a two-step sintering method. The effects of MgO on microstructures and luminescent properties of GAGG:Ce TCPs are investigated for the first time. For the optimized Mg²⁺ of x = 0.5%, the in-line transmittance of the obtained TCP reaches 78.6%. Performances of the titled TCPs in high-power light-emitting diodes (LEDs) and laser diodes (LDs) lighting are illustrated. The optimized TCP shows the luminous efficacy of 84.0 lm W^?1 in LD lighting. This work provides a strategy to modify TCPs for the next-generation LD lighting.     

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.     

Structural properties and mechanical behavior of SWCNTs and MWCNTs reinforced Al2O3 fabricated by spark plasma sintering

Carbon nanotubes due to their structural and mechanical properties are good candidates as the second phase to improve the mechanical properties of alumina-based ceramics. In the present study, the effects of single wall and multi-wall carbon nanotubes on structural and mechanical properties of alumina were investigated. SWCNTs and MWCNTs were dispersed in alumina powder via a conventional method using 1 wt % PVA water solution as media. Sintering process for two different composite powders, alumina-2 wt. % SWCNTs and alumina 2 wt % MWCNTs was performed by spark plasma sintering technique at 1500 °C and 20 MPa for 10 min. Results showed that the presence of CNTs in alumina caused a considerable amount of porosity in final bodies. SEM images of fracture surfaces revealed the agglomeration of SWCNTs which played a dominant role in the deterioration of mechanical properties. MWCNTs reinforced alumina obtained higher Vickers hardness and bending strength values (12.91 GPa and 291 MPa, respectively) compared to that of SWCNTs (9.18 GPa and 276 MPa, respectively), due to sever agglomerate of SWCNTs throughout sintered composites. Typical load-displacement (P/h) curves were obtained from bending strength test and discussed. It was concluded that the addition of MWCNTs to alumina represented better densification and mechanical properties compared to SWCNTs.     

Synthesis and characterization of Al2O3-TiC-ZrO2 ceramics with intragranular nanostructure by spark plasma sintering

In this paper, Al₂O₃-TiC ceramic composites with intragranular nano-ZrO₂ were prepared in vacuum by spark plasma sintering (SPS). The effect of ZrO₂ particles with different nano-sizes on the microstructure and mechanical properties of ceramics was studied. The results show that SPS can achieve relative densification of materials without generating new impurity phases. At the same time, the sintering densification temperature of ceramic materials can be reduced by adding ZrO₂ (20 nm) particles. Under the action of SPS strong electric field, the nano-ZrO₂ adsorbed on the surface of the matrix particles can enter the interior of matrix grains, and form intragranular nanostructures when the grain boundaries move and the particles merge. The microstructure and mechanical properties of ceramic materials can be improved through the intragranular structure formed by nanoparticles. The main reasons for the increased strength and toughness of ceramic materials are crack deflection, crack bridging and transgranular fracture.     

Fabrication of transparent Y2O3 ceramics by two-step spark plasma sintering

Transparent Y₂O₃ ceramics were successfully fabricated by spark plasma sintering applying a two-step pressure and heating profile. Through the shrinkage curve of the single-step SPS profile, it was confirmed that shrinkage occurred at 800°C–1250°C, and it was selected as the two-step pressure profile. After the first-step SPS stage at 1250°C, the second-step SPS stage, which had the highest real in-line transmittance, was completed at 1500°C. The two-step SPS profile improved the shrinkage behavior and was able to achieve sufficient densification without excessive coarsening. As a result, the normalized real in-line transmittance to 1 mm was 80.6% at 1100 nm, which is close to the theoretical transmittance of 81.6%. The two-step pressure and heating profile in the SPS process was a significant advantage in manufacturing ceramics that were transparent and had sufficient densification.     

Direct tape casting of Al2O3/AlN slurry for AlON transparent ceramic wafers via one-step reaction sintering

In this work, transparent aluminate oxynitride (AlON) ceramic wafers were successfully fabricated by the direct non-aqueous tape casting of Al₂O₃/AlN slurry and the one-step reaction sintering for the first time. The reaction sintered AlON ceramic wafer exhibits high transmittance of 73.2 % at the wavelength of 1600 nm. This fabricating route realizes smooth and flexible tape without cracks or pinholes in Al₂O₃/AlN system and efficiently shortens the preparation cycle of transparent AlON wafers, which is a feasible way to prepare high-quality transparent AlON ceramics with large lateral sizes and thin thicknesses by reaction sintering, might also promote the application of transparent AlON ceramic wafers.     

Microstructure and properties of Al2O3–TiC nanocomposites fabricated by spark plasma sintering from high-energy ball milled reactants

In situ synthesis of Al₂O₃–TiC nanocomposite powders from a mixture of titanium, graphite, and Al₂O₃ powders by high-energy ball milling (HEBM) and its consolidation through spark plasma sintering (SPS) were investigated. After being milled for 25 h at ambient temperature, the powder mixtures were mainly composed of homogeneous nanosized Al₂O₃ particle and amorphous TiC solid solution. The relative density of the samples consolidated by SPS technique in vacuum at 1480 °C for 4 min reached 99.2%. The final products exhibited very fine microstructure, and the grain sizes of Al₂O₃ and TiC were about 400 nm and 200 nm, respectively, with a flexure strength of 944 ± 21 MPa, Vickers hardness 21.0 ± 0.3 GPa, fracture toughness 3.87 ± 0.2 MPa m^1/2, and electrical conductivity 1.2787 × 10⁵ S m⁻¹.