Highly-doped YAG:Sm3+ transparent ceramics: Effect of Sm3+ ions concentration

YAG:Sm³⁺ (3–15 at.%) transparent ceramics, a promising cladding material for suppressors of parasitic oscillations at 1064 nm of YAG:Nd³⁺ lasers, have been prepared by solid-state reactive sintering at 1725 °C. The effect of samarium ions concentration on the microstructure and optical properties of YAG:Sm³⁺ sintered ceramics was studied for the first time. The solubility limit of samarium ions in the garnet matrix was found to lie within the range of 9–11 at.%. The spectroscopic characterization of YAG:Sm³⁺ (3–15 at.%) ceramic samples showed that the absorption coefficients corresponding to Sm³⁺ ions transitions increased linearly with increasing Sm³⁺ doping. Also, the increase in the concentration of Sm³⁺ ions contributes to the increase in the intensities of the satellites, leading to the broadening of the main spectral lines and implicitly to the increase of the absorption coefficient around 1064 nm. It was shown that YAG:Sm³⁺ ceramics doped with 9 at.% Sm³⁺ ions possess optical losses of 0.07 cm^?1 at 808 nm and an optical absorption coefficient of 4.45 cm^?1 at 1064 nm. The concentration dependence of the ⁴G_5/2 level decay confirmed that the luminescence extinction is due to the energy transfer between the Sm³⁺ ions through cross-relaxation processes. All these results show that highly-doped YAG:Sm³⁺ (9 at.%) ceramics could be the best candidate for parasitic oscillation suppression in high-power YAG:Nd³⁺ lasers at 1064 nm.     

Synthesis of Nd:YAG powders leading to transparent ceramics: The effect of MgO dopant

Neodymium doped yttrium aluminum garnet (Nd:YAG) ultrafine powders were synthesized by co-precipitation method using MgO as dopant. The addition of small amount of MgO can reduce the agglomeration and particle size of the produced Nd:YAG powders. The results show that pure phase YAG powders can be achieved by calcining of the precursors at 1000 °C for 2 h. The MgO doped Nd:YAG powders show better dispersion compared with the undoped powders. When the MgO content is 0.01 wt.%, well-dispersed Nd:YAG powders with spherical particles of 100 nm diameter were obtained. The transmission of the corresponding Nd:YAG ceramics is 82.6% at the wavelength of 1064 nm, which is comparable to Nd:YAG single crystals.     

Fabrication and laser behaviors of Nd:YAG ceramic microchips

Transparent Nd:YAG ceramic microchips were fabricated through the slip casting shaping directly from the slurry formed by the commercial Al₂O₃/Y₂O₃/Nd₂O₃ powders, and followed by the vacuum sintering procedure. Viscosity of the slurries, the phase evolution and the densification behavior were investigated. For the Al₂O₃/Y₂O₃/Nd₂O₃ compound slurries system, the optimal condition is 0.5 wt.% NH₄PAA dispersant and 30 wt.% solid loading at pH ≥ 8. The YAG phase started to form at 1250° C and pure YAG phase could be obtained at 1400° C. The optical in-line transmittance of the Nd:YAG ceramics with thickness of 2 mm was about 83.8% at 1064 nm and 82.5% at 400 nm, which hit the upper limit of the theoretically calculated value. For the 1.0 at.% Nd:YAG ceramic microchip, the slope efficiency was 43% for 1.0 at.% Nd:YAG ceramic pumped by 920 mW cw Ti:sapphire tunable laser, and the maximum laser output power 246 W was obtained for 2.0 at.% Nd:YAG ceramics pumped by 925 W LD.     

Synthesis,consolidation and dielectric properties of BLT ceramics processed by M-PVA gel ignition technique

Abstract

Abstract

Polycrystalline samples of lanthanum modified bismuth titanate ceramics with composition Bi_3·25La_0·75Ti₃O₁₂ (BLT) were prepared at three different sintering temperatures (1050, 1100 and 1150°C) using M-PVA gel ignition technique. The samples were characterised for structural and electrical properties. A significant amount of as burnt BLT powder was found to be crystalline in nature having a yellowish colour. Very fine BLT nanoparticles were characterised by TEM analysis. Single phase with orthorhombic crystal structure was observed for all the samples, confirmed by X-ray analysis. Dielectric properties were studied as a function of frequency and temperature. More than 95% relative density was observed for all the three sintered samples. The sample sintered at 1100°C showed highest dielectric constant and relative density and lowest loss.     

The red-emitting phosphors of Mn4+-activated A2MgWO6 (A = Ba,Sr, Ca) for light emitting diodes

A series of Mn⁴⁺ ions activated A₂MgWO₆ (A = Ba, Sr, Ca) phosphors, showing bright red emission peaks appeared around 700 nm under the excitation of 355 nm, were synthesized by the solid-state reaction. The crystal structures and photo-luminescent (PL) properties of these synthesized phosphors were deeply investigated with the aids of X-ray diffraction measurement (XRD), and the temperature dependent PL/decay curves in detail. The optimum doping concentration of Mn⁴⁺ ions in A₂MgWO₆ (A = Ba, Sr, Ca) lattices were studied through the relationship between the Mn⁴⁺ ions doping concentrations and the luminescent intensities. The thermal stability of the synthesized red-emitting phosphors was checked based on the temperature-dependent PL intensities ranging from 7 to 510 K. Comparative studies of the luminescent properties for Mn⁴⁺ ions in isostructural A₂MgWO₆ (A = Ba, Sr, Ca) lattice with double perovskite structure were studied. The results indicate that the synthesized red-emitting phosphors are the ideal choice for white light emitting diodes (W-LEDs).     

Fatigue-resistant,temperature-insensitive strain behavior and strong red photoluminescence in Pr-modified 0.92(Bi0.5Na0.5)TiO3–0.08(Ba0.90Ca0.10)(Ti0.92Sn0.08)O3 lead-free ceramics

An electric-field-induced large strain and strong photoluminescence was achieved by introducing trivalent Pr³⁺ as the activator into 0.92(Bi_0.5Na_0.5)TiO₃ − 0.08(Ba_0.90Ca_0.10)(Ti_0.92Sn_0.08)O₃ (BNT−8BCST) ceramics. Around a critical composition of 0.4 mol% Pr³⁺, a large strain of ∼0.39% with a relatively small hysteresis compared with existing lead-free Bi-perovskite ceramics was obtained. In particular, the strain is very resistant to field cycling and thermal shock, giving the materials attractive for its exceptionally good fatigue resistance and high temperature stability. Besides the excellent electrical properties, Pr³⁺-modified BNT−8BCST host exhibits a strong photoluminescence with a bright red emission at 610 nm assigned to ¹D₂ → ³H₄ transitions of the Pr³⁺ ions upon a blue light excitation of 400–500 nm. The photoluminescence can be enhanced through poling treatment of the samples. Moreover, samples have a superior water resistance property which almost maintaining the same photoluminescence intensity after 40 h water immersion time. These results suggest the material may have potential application as a multifunctional device such as “on-off” actuator and electric field-controlled photoluminescence devices by integrating its excellent luminescence and electrical properties.     

Fabrication of Sn doped Ba(Mg1/3Ta2/3)O3 transparent ceramics by a solid state reaction method

Transparent disordered BMT ceramics were obtained by solid state reaction. Sn⁴⁺ ions were incorporated to make the B site of the perovskite structure disordered. The stoichiometric powder mixture with and without Sn doping was calcinated at 1300 °C, respectively and they were both characterized. After dry pressing, the pellets with Sn doping were sintered at 1600 °C in oxygen atmosphere for 4 h. The grain size of the transparent ceramics is around 12 μm. No pores were detected in or among the grains. The inline transmittance of the material is 66% at 580 nm. The refractive index is 2.09 at 1600 nm.     

Solid-state pressureless sintering of silicon carbide below 2000 °C

To date, solid-state pressureless sintering of silicon carbide powder requires sintering aids and high sintering temperature (>2100 °C) in order to achieve high sintered density (>95% T.D.). Two-step sintering (TSS) method can allow to set sintering temperature lower than that conventionally required. So, pressureless two-step sintering process was successfully applied for solid-state sintering (boron carbide and carbon as sintering additives) of commercial SiC powder at 1980 °C. Microstructure and mechanical properties of TSS-SiC were evaluated and compared to those obtained with the conventional sintering (SSiC) process performed at 2130 °C. TSS-SiC showed finer microstructure and higher flexural strength than SSiC with very similar density (98.4% T.D. for TSS-SiC and 98.6% T.D. for SSiC).     

Effect of annealing process on IR transmission and mechanical properties of spark plasma sintered Yttria

In this study, fully dense Yttria ceramics were successfully fabricated by spark plasma sintering (SPS) at temperatures of 1300 and 1350 $℃$. The effects of post-annealing on IR transmission were investigated by Fourier transform infrared spectroscopy (FTIR) at various temperatures ranging from 1050 to 1250 $℃$. It was found that the optimum annealing temperature depends strongly on the sintering temperature. Annealed samples showed white opaqueness mainly due to the increase and coalescence of pores after annealing and showed an absorption band around 6.6 $\mu m$ which limits usage of yttria in IR applications. Sintering at 1350 $℃$ and annealing at 1250 $℃$ led to the maximum IR transmittance above 80% at wavelength of 5 $\mu m$ for a 3.5-mm-thick sample. The hardness and the fracture toughness of the samples were analyzed in detail and hardness of 9.2 GPa and fracture toughness of 1.65 MPa m^1/2 were obtained for the above sample.     

The effect of SiC addition on photoluminescence of YAG:Ce phosphor for white LED

An effective way of improving photoluminescence (PL) of YAG:Ce by addition of small amount of SiC and sintering in air was described. The breakdown of SiC during sintering process in air was employed to provide the presence of SiO₂ and CO both of which are known to be beneficial in enhancing the PL of YAG:Ce phosphor. SiC in the form of a fine powder was added to YAG:Ce powder and sintered to densities of >99% of theoretical density. The highest luminescence was measured in sample containing 0.08?wt% SiC. The effect of the formed SiO₂ and CO was discussed and their contribution to the emission intensity was assessed. The enhancement of PL intensity is attributed to the formation of vacancies, both on Y sub-lattice and on oxygen sub-lattice and their ability to release the electrons for subsequent reduction of Ce⁴⁺ to Ce³⁺ which plays a role of luminescence activator.     

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.     

Optical and mechanical properties of Mg-doped sialon composite with La2O3 as additive

Using 0.5 wt.% La₂O₃ as a sintering additive, Mg-doped sialon composite with the maximum infrared transmittance of 50% was fabricated by hot pressing at 1800 °C. The addition of La₂O₃ significantly promotes the densification process of Mg-doped sialon and the anisotropic growth of β-sialon grains. As a result, the sintered material exhibits high hardness (20.2 GPa), fracture toughness (4.8 MPa m^1/2) and flexural strength (664 MPa). Furthermore, the nano-sized glassy phases concentrated at triple junctions have no obviously negative impact on infrared translucency of Mg-doped sialon.     

Low temperature synthesis of YAG:Ce phosphors by LiF assisted sol-gel combustion method

Ce doped yttrium aluminium garnet (YAG:Ce) was synthesized by LiF assisted sol-gel combustion method. The thermal behavior, composition, and microstructure feature of the precursor were studied by TG/DTA, XRD, PL, and SEM. The using of LiF in the sol-gel combustion process was helpful to decrease the sintering temperature about 200 °C. The X-ray diffraction patterns of the powder sintered at 540 °C were identical with the stoichiometric YAG composition, which was the lowest temperature reported for the synthesis of crystalline and single phase YAG. The PL intensity of the particles was found to be affected by the content of LiF and this phenomenon was thought to be related to the change of phase composition with the increase of flux.     

CHARACTERIZATION OF CERIUM-DOPED YTTRIUM ALUMINIUM GARNET NANOPOWDERS SYNTHESIZED VIA SOL-GEL PROCESS

In this work the sol-gel process was used to prepare Ce-doped yttrium aluminium garnet (Y ₃ A l ₅ O ₁₂, YAG) samples. The synthesis products were characterized by infrared spectroscopy (IR), X-ray powder diffraction analysis (XRD), and transmission electron microscopy (TEM). The particle size and luminescence properties of synthesized samples were also determined. The XRD patterns of Y ₃ A l ₅ O ₁₂:Ce samples showed that phase purity of garnets depends on the synthesis temperature and concentration of dopant. The YAG:Ce samples calcined at 1000°C showed the formation of single-phase YAG in the whole doping range (from 0 up to 10 mol% of Ce). However, during calcination at 1300°C the formation of CeO₂ as an impurity phase at >4 mol% of Ce was observed. The mean particle size of Y ₃ A l ₅ O ₁₂:Ce sample (4 mol% of Ce) synthesized at 1300°C was determined to be approximately 180–280 nm. The luminescence properties of Ce-doped YAG also depend on cerium concentration in the samples. The highest emission (λ _ex  = 450nm) intensity was determined for Y ₃ A l ₅ O ₁₂:Ce samples doped by 5–6 mol% of Ce.