Aqueous slip casting of transparent yttrium aluminum garnet (YAG) ceramics

Transparent YAG ceramics were prepared by slip casting an aqueous dispersed mixture of commercial Al₂O₃ and Y₂O₃ powders. The powders were co-dispersed with poly(acrylic acid) and citric acid. Polyethylene glycol of 0.5 wt.% (PEG 4000) and 0.5 wt.% tetraethyl orthosilicate were added as binder and a sintering aid, respectively. Dried samples were vacuum sintered at 1800 °C for 16 h. In general, YAG ceramics cast from Newtonian suspensions were optically transparent and had optical transmittances >80% from 340 to 840 nm. Slightly flocculated dispersions, as evidenced by higher viscosity and non-Newtonian rheology, resulted in translucent samples with large pores and lower optical transmittances.     

Co-precipitation synthesis route to yttrium aluminum garnet (YAG) transparent ceramics

Yttrium aluminum garnet (YAG) precursor was synthesized via a coprecipitation method with aluminum nitrate and yttrium nitrate as raw materials, using ammonium hydrogen carbonate (AHC) as the precipitant. Fine and low-agglomerated YAG powder was obtained by calcining the precursor at 1200 °C. The primary crystallites were measured to be ～120 nm in size and weakly agglomerated to a particle size of ～500 nm, indicating a high degree of sinterability. With 0.5 wt% tetraethyl orthosilicate (TEOS) and 0.1 wt% magnesia as sintering aids, transparent YAG ceramics were fabricated by vacuum sintering at 1730–1790 °C for various hours. The influences of sintering temperature and holding time on the microstructure and transmittance of YAG ceramics were discussed.     

Structure formation in yttrium aluminum garnet (YAG) fibers

Polycrystalline yttrium aluminum garnet (YAG, Y₃Al₅O₁₂) fibers were prepared from aqueous solutions of aluminum chlorohydrate and yttrium chloride. Fiber processing was accomplished via dry spinning. Poly(vinylpyrrolidone) (PVP) was used as spinning aid. Polycrystalline YAG fibers were obtained by pyrolysis of the green fibers followed by sintering at defined temperatures in air. Ceramic fibers were 9–16 μm in diameter. Differential scanning calorimetry/thermogravimetric analysis coupled with mass spectrometry (DSC/TGA-MS) showed an exothermic peak at 920 °C assigned to the crystallization of YAG and an overall ceramic yield of 38% at 1400 °C. X-ray diffraction (XRD) analysis showed that phase-pure YAG can be obtained at 1600 °C after intermediate formation of Y₂O₃ and monoclinic yttrium aluminum oxide (YAM, Y₄Al₂O₉) phases.     

Densification of transparent yttrium aluminum garnet (YAG) by SPS processing

Nano-size YAG powder co-mixed with 0.25 wt.% LiF was used to fabricate transparent polycrystalline YAG specimens by means of the Spark Plasma Sintering (SPS) technique. The presence of the LiF additive in the initial nano-powder allows obtaining fully dense disc shaped (up to 4 mm thick) transparent specimens at the outcome of a 2 h treatment at 1300 °C. The presence of LiF plays a key role in the mass transport related effects during the densification of YAG to full density and also in the elimination of the residual carbon contamination, allowing reaching a level of optical transmittance close to the theoretical value.     

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.     

Co-precipitation synthesis and sintering of yttrium aluminum garnet (YAG) powders: the effect of precipitant

YAG precursors were co-precipitated from a mixed solution of aluminum and yttrium nitrates using ammonia water and ammonium hydrogen carbonate as precipitants, respectively. Phase evolution of the precursors during calcination and sinterability of the resultant YAG powders were compared between the two methods. The use of ammonia water produced a hydroxide precursor with an approximate composition of Al(OH)₃·0.3[Y₂(OH)₅(NO₃)·3H₂O] which transformed to pure YAG at about 1000°C via YAlO₃ phase. Severe agglomeration caused poor sinterability of the resultant YAG powders. The use of ammonium hydrogen carbonate produced a carbonate precursor with an approximate composition of NH₄AlY_0.6(CO₃)_1.9(OH)₂·0.8H₂O. The precursor directly converted to pure YAG at about 900°C. The precursor was loosely agglomerated and the resultant YAG powders showed good dispersity and excellent sinterability. For the same calcination temperature of 1100°C, YAG powders from the hydroxide precursor and the carbonate precursor densified to ∼81.2 and ∼99.8% of the theoretical, respectively, by vacuum sintering at 1500°C for 2 h.     

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.     

Erbium-doped LAS glass ceramics prepared by spark plasma sintering (SPS)

Dense nanocrystalline glass ceramics of the Li₂O–Al₂O₃–SiO₂ (LAS) system were obtained by spark plasma sintering (SPS) of powders prepared by sol–gel method. The low thermal expansion LAS glass ceramic was chosen as host matrix for erbium ions. ZrO₂ was added both as a nucleating agent and as a possible good environment for the rare earth. The developed crystalline phases were analysed by X-ray diffraction (XRD) and the amorphous phase was quantified. Scanning and transmission electron microscopy (SEM, TEM) was used to investigate the microstructure. A different behaviour during the crystallisation process was observed between the sample prepared through the sintering of powders and the glass produced by the melting technique. A photoluminescence characterisation was also performed.     

Ultraviolet emission transparent Gd:YAG ceramics processed by solid-state reaction spark plasma sintering

Transparent 1% Gd-doped YAG and YAG ceramics were synthesized via solid-state reaction spark plasma sintering using commercially available powder and TESO as a sintering additive. The highest in-line transmission values achieved were 77.1% at 550 nm and 80.6% at 800 nm in the 1% (at.%) Gd-doped YAG transparent ceramic with 99.90% relative density. Ultraviolet emission at 312.5 nm was observed in 1% Gd-doped YAG ceramic via photoluminescence excitation, making it a promising material for applications in solid-state UV devices.     

BiFeO3 ceramics synthesized by spark plasma sintering

Phase-pure BiFeO₃ particles were synthesized by an improved solid state technique. High density BiFeO₃ ceramics were prepared using these particles by spark plasma sintering (SPS). The dielectric permittivity and loss of SPS samples were measured as functions of sintering temperature, frequency, and annealing conditions. Dielectric spectra of the ceramics annealed at 650 °C were characterized in a broad range of temperature (300–725 K) and frequency (100 Hz to 20 MHz). Two kinds of dielectric relaxation following the Arrhenius law were detected in low and high temperature ranges, respectively. The low temperature dielectric relaxation could be almost completely removed by annealing in vacuum and it should be assigned to be a valence fluctuation of Fe ions, while the high temperature dielectric relaxation was proposed to stem from the short-range motion of oxygen vacancies.     

Transparent hydroxyapatite ceramics with nanograin structure prepared by high pressure spark plasma sintering at the minimized sintering temperature

A hydrothermally processed bulky powder composed of loosely aggregated nano-sized rods was consolidated by spark plasma sintering. The use of a high pressure cell allows the application of pressure up to 500 MPa. It was found that applying of high pressure is beneficial for widening up the kinetic window for attaining dense HAp nanoceramics. The high transparency of HAp nanoceramics obtained in this study is ascribed to the high density and homogeneous nano-grained structure achieved besides the unique intrinsic optical properties of the HAp crystal itself, i.e. its low refractive index and very small birefringence. Achieving full densification at the minimized sintering temperature allows for the first time the preparation of transparent HAp nanoceramics with stoichiometric composition, i.e. avoiding the loss of structural water that commonly takes place during the conventional ways of sintering.     

Effect of sintering temperature on the transparency and mechanical properties of lutetium aluminum garnet fabricated by spark plasma sintering

Transparent lutetium aluminum garnet (Lu₃Al₅O₁₂, LuAG) was fabricated by reactive spark plasma sintering. The effect of sintering temperature on the crystal phase, microstructure, transparency and mechanical properties of LuAG bodies was investigated. Fully dense and single-phase LuAG bodies were obtained at sintering temperatures 1573–1923 K. The average grain size increased from 0.18 to 0.52 μm with increasing sintering temperature from 1573 to 1773 K, and grain growth became significant at 1823 K. Transmittance showed a maximum value of 77.8% at 2000 nm at a sintering temperature of 1773 K after annealing at 1423 K in air for 43.2 ks. The Vickers hardness increased from 14.2 to 17.2 GPa with decreasing grain size from 7.45 to 0.23 μm.     

Translucent LiSr4(BO3)3 ceramics prepared by spark plasma sintering

Lithium borates are promising materials for thermal neutron detection. However, a strong tendency of borates for glass transformation can lower the detection efficiency of some luminescence centres. Here, we describe the synthesis of well-crystalline translucent borate ceramics. The precursor powder of undoped LiSr₄(BO₃)₃ was prepared using a wet homogenization method and then densified to ceramic pellets at different sintering temperatures using SPS. As the sintering temperature increased, the degree of densification and crystallite connectivity improved, rendering the prepared pellets translucent.     

Transparent ultrafine Yb3+:Y2O3 laser ceramics fabricated by spark plasma sintering

Conventional ceramic processing techniques do not produce ultrafine‐grained materials. However, since the mechanical and optical properties are highly dependent on the grain size, advanced processing techniques are needed to obtain ceramics with a grain size smaller than the wavelength of visible light for new laser sources. As an empirical study for lasing from an ultrafine‐grained ceramics, transparent Yb³⁺:Y₂O₃ ceramics with several doping concentrations were fabricated by spark plasma sintering (SPS) and their microstructures were analyzed, along with optical and spectroscopic properties. Laser oscillation was verified for 10 at.% Yb³⁺:Y₂O₃ ceramics. The laser ceramics in our study were sintered without sintering additives, and the SPS produced an ultrafine microstructure with an average grain size of 261 nm, which is about one order of magnitude smaller than that of ceramics sintered by conventional techniques. A load was applied during heating to enhance densification, and an in‐line transmittance near the theoretical value was obtained. An analysis of the crystal structure confirmed that the Yb³⁺:Y₂O₃ ceramics were in a solid solution. To the best of our knowledge, this study is the first report verifying the lasing properties of not only ultrafine‐grained but also Yb‐doped ceramics obtained by SPS.     

Transparent yttria stabilized zirconia from glycine-nitrate process by spark plasma sintering

Nanosized cubic yttria-stabilized zirconia (ZrO₂-8 mol% Y₂O₃) powder was synthesized via a glycine-nitrate process combining with high-energy ball milling. Effect of the calcination temperature on the sintering activity of the powders was discussed. The present investigations demonstrated the most favorable calcination temperature was 900 °C for obtaining fine nanopowders with high sinterability. Consolidation of the nanopowder was carried out by spark plasma sintering at 1200-1350 °C for 5 min. Transparent ceramics fabricated could be achieved at 1300 °C. Optical transmittance calculation based on Mie theory fits well with the experimental results of the transparent specimen sintered at 1300 °C, while the inconsistence for the specimen sintered at 1350 °C above 600 nm might be attributed to the scattering by grain boundaries and higher oxygen vacancy content.     

Bulk boron carbide nanostructured ceramics by reactive spark plasma sintering

Bulk boron carbide (B₄C) ceramics was fabricated from a boron and carbon mixture by use of one-step reactive spark plasma sintering (RSPS). It was also demonstrated that preliminary high-energy ball milling (HEBM) of the B+C powder mixture leads to the formation of B/C composite particles with enhanced reactivity. Using these reactive composites in RSPS permits tuning of synthesized B₄C ceramic microstructure. Optimization of HEBM + RSPS conditions allows rapid (less than 30 min of SPS) fabrication of B₄C ceramics with porosity less than 2%, hardness of ~35 GPa and fracture toughness of ~ 4.5 MPa m ^1/2     

Fabrication of sub-micrometer MgO transparent ceramics by spark plasma sintering

Transparent MgO ceramics were fabricated by spark plasma sintering (SPS) of the commercial MgO powder using LiF as the sintering additive. Effects of the additive amount and the SPS conditions (i.e., sintering temperature and heating rate) on the optical transparency and microstructure of the obtained MgO ceramics were investigated. The results showed that LiF facilitated rapid densification and grain growth. Thus, the MgO ceramics could be easily densified at a moderate temperature and under a low pressure. In addition, the transparency and microstructure of the MgO ceramics were found to be strongly dependent on the temperature and heating rate. For the MgO ceramics sintered at 900 °C for 5 min with the heating rate of 100 °C/min and the pressure of 30 MPa from the powders with 1 wt% LiF, the average in-line transmittance reached 85% in the range of 3 – 5 μm, and the average grain size is ∼0.7 μm.     

Gel-casting of transparent magnesium aluminate spinel ceramics fabricated by spark plasma sintering (SPS)

In this paper, a transparent magnesium aluminate spinel ceramic was fabricated through the newest colloidal gel casting method, using a synthetic powder with the average particle size of 90 nm and Isobutylene-Maleic Anhydride (ISOBAM) additive. ISOBAM served as both a dispersant and a gelation agent to achieve a dense body. Also, the suspension rheological behavior was optimized by the solid loading of 85 wt%, the additive content of 0.7 wt%, and the gelation time of 350 s. This led to a green body with a density equal to 65% of theoretical density and the green strength of 14.48 MPa. The results revealed that the reduction of porosity and the uniform distribution of pores in the green body (smaller than half of the initial powder particle size, 35 nm), as accompanied by spark plasma sintering (SPS), resulted in the final body density of 99.97%, as well as the high in-line transmittance of 86.7% at the wavelength of 1100 nm.