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.     

YAG ceramic processed by slip casting via aqueous slurries

Stable YAG (Y₃Al₅O₁₂) aqueous slurry with ammonium polyacrylate (NH₄PAA) polyelectrolytes as dispersant was prepared by ball mill method. The effects of polyelectrolyte concentration and pH value on the stability of the suspension is described here, and the stability maps are constructed at different pH value and polymer concentration. The rheological behavior of YAG slips of different solid loading (60–70%) has been studied by measuring their viscosity and shear stress as a function of shear rate and pH of the slurry. An optimal amount of dispersant and pH value for the suspension was found. YAG suspension displays a maximum in zeta potential values and a minimum viscosity in pH range of 9–11. Slips behaved as near Newtonian at the pH value up to a solid loading of 60 wt% and as non-Newtonian with thixotropic behaviors above this solid loading value. The density and the green as well as sintered microstructure of the cast products bear a direct relationship to the state of this slips induced by the alternation in the pH and the concentration of the dispersant as well as solid loading.     

Preparation of spray-dried powders leading to Nd:YAG ceramics: The effect of PVB adhesive

The mixed powders were obtained with Al₂O₃, Y₂O₃ and Nd₂O₃ powders as starting materials using spray drying technology. The main purpose of introducing polyvinyl butyral (PVB) is to contribute to spray granulation of the powders and inhibition of the compositions segregation. The effect of the addition of PVB (0, 1, 2, and 3 wt%) on the morphologies and compositions of the spray-dried powders is discussed. When calcined at 1000 °C for 2 h, the powders with PVB as an adhesive show sphericity and better dispersion. No compositions segregation can be detected. It is found that the powders with 2 wt% PVB after calcinations are suitable for the fabrication of Nd:YAG transparent ceramics. The corresponding ceramics consists of a well-defined microstructure, and no pores or other defects are observed.     

Compressive mechanical properties of partially sintered porous alumina of bimodal particle size system

This paper examined theoretically and experimentally packing behavior, sintering behavior and compressive mechanical properties of sintered bodies of the bimodal particle size system of 80 vol% large particles (351 nm diameter)–20 vol% small particles (156 nm diameter). The increased packing density as compared with the mono size system was explained by the packing of small particles in 6-coordinated pore spaces among large particles owing to the similar size relation between 6-coordinated spherical pore and small particle. The sintering between adjacent large particles dominated the whole shrinkage of the powder compact of the bimodal particle size system. However, the bimodal particle size system has a high grain growth rate because of the different curvatures of adjacent small and large particles. The derived theoretical equations for the compressive strengths of both mono size system and bimodal particle size system suggest that the increase in the grain boundary area and relative density by sintering dominate the compressive strength of a sintered porous alumina. The experimental compressive strengths were well explained by the proposed theoretical models. The strength of the bimodal particle size system was high at low sintering temperatures but was low at high sintering temperatures as compared with that of mono size system of large particles. This was explained by mainly the change of grain boundary area with grain growth. The stress–strain relationship of the bimodal particle size system showed an unique pseudo-ductile property. This was well explained by the curved inside stress distribution along the sample height. The inside stress decreases toward the bottom layer. The fracture of one layer of sintered grains over the top surface proceeds continuously with compressive time along the sample height when an applied stress reaches the critical fracture strength.     

Temperature dependence of piezoelectric properties on Nd and V co-substituted Bi4Ti3O12 ceramics for ceramic resonator applications

The temperature dependences of the piezoelectric properties of (Bi_4−yNd_y)_1−(x/12)(Ti_3−xV_x)O₁₂ [BNTV-x, y (x = 0.01, y = 0.00–1.00)] were investigated for environmentally friendly lead-free piezoelectric ceramic resonators with low-temperature coefficients of resonance frequency, TC-f. The |TC-f| in the (33) mode improved with increasing concentration of modified Nd ions, y, and exhibited the smallest |TC-f| value of 77.4 ppm/°C at y = 0.75 (BNTV-0.75). The |TC-f| in the other vibration mode (t), was also investigated for the BNTV-0.75 ceramic, and a smaller value of 42 ppm/°C was obtained. The (t) mode of the BNTV-0.75 ceramic showed excellent piezoelectric properties: Q_m = 4200, Q_e max = 31 and TC-f = −49.8 ppm/°C. These properties are very similar to those of commercialized hard PZT ceramics for resonator applications. The BNTV-0.75 ceramic seems to be a superior candidate material for lead-free piezoelectric applications of ceramic resonators.     

Synthesis, growth mechanism and photoluminescence of monodispersed cubic shape Ce doped YAG nanophosphor

In the present work, a novel method for the synthesis of monodispersed cubic shape Ce-doped yttrium aluminum garnet (YAG:Ce) nanophosphors is reported. Single phase Ce doped YAG nanoparticles are prepared by solvothermal processing, followed by annealing treatment. Morphological investigation by scanning electron microscopy (SEM) showed the formation of monodispersed 500 nm cubic shape Ce-doped YAG phosphor. The crystalline Ce-doped YAG showed broad emission peaks in the range of 480-640 nm with maximum intensity at 524 nm. The emission intensity increased with increase in calcination temperatures while reduced with increase in Ce³⁺ ions concentration. Detailed study was carried out to understand the formation of monodispersed cubic shape Ce doped YAG nanoparticles. It was found that the solvent, surfactant and impurity (counter ions of cerium and aluminum salt) has significant effect on the crystal growth.     

Fabrication and kW-level MOPA laser output of planar waveguide YAG/Yb:YAG/YAG ceramic slab

Using the tape casting method combined with vacuum sintering and hot isostatic pressing, high-quality planar waveguide YAG/10 at.%Yb:YAG/YAG ceramics were successfully prepared. For the sample presintered at 1750°C for 30 hours and then HIPed at 1700°C for 3 hours in 200 MPa argon, the in-line transmittance reached 82.5% at 400 nm and the average grain size was ~17.1 μm. The diffusion behaviors of Yb ions across the contact boundary between the cladding YAG layer and the core Yb:YAG layer were determined by Fick's second law. Then, a 1030 nm continuous-wave (CW) Yb:YAG planar waveguide ceramic laser based on the structure of master oscillator power amplification (MOPA) was realized. After a single-pass amplification, the maximum output of the ceramic slab (60 × 10 × 1 mm³) reached 1251 W and the corresponding optical-to-optical efficiency was 30.0%, which is the highest output power of a Yb:YAG planar waveguide ceramic laser to the best of our knowledge.     

Influence of solid loading on the rheological,porosity distribution,optical and the microstructural properties of YAG transparent ceramic

Stable aqueous dispersed mixture of commercial Al₂O₃ and Y₂O₃ nano powders was prepared by ball mill. Ammonium poly meta acrylate (Dolapix CE64) and tetraethyl orthosilicate (TEOS) were added as dispersant and sintering aid, respectively. The effects of slurry solid loading on the fabrication of transparent polycrystalline YAG ceramics by slip casting method were investigated. The rheological properties of slurries with different solid loading (64, 70 and 76?wt%) were studied by measuring the viscosity and shear stress as a function of shear rate. The effect of solid loadings on the porosity distribution was examined. The specimens were vacuum-sintered at 1715?°C for 10?h. Slips with 64 and 70?wt% solid loading behaved as near-Newtonian and as non-Newtonian with thixotropic behavior at 76?wt% solid loading. The relative densities of the green bodies increased from 58.0?±?0.6% (SD?=?0.424) to 64.0?±?0.3% (SD?=?0.228) by increasing the solid loading from 64?wt% to 70?wt% and then decreased to 63.0?±?0.2% (SD?=?0.141) at 76?wt% solid loading. The results showed that the suitable solid loading for fabricating transparent YAG ceramics is 70?wt%. This sample had the narrowest pore size distribution (4–100?nm), homogenized surface fracture of green body, dense microstructure (99.990?±?0.005% final relative density, SD?=?0.003) and the average grain size of 6?µm. It had the highest in-line transmittance, which was approximately 77% at 1064?nm.     

Microstructure and optical properties of Nd: YAG transparent ceramics with the addition of Lu3+ ions

The Nd:YAG transparent ceramics with addition of Lu³⁺ ions were fabricated by co-precipitation method and vacuum sintering. Pure YAG phases were obtained when Lu³⁺ ion content was kept under 4.5?at.-%. Lattice constant of polycrystalline ceramic with 0.8?at.-% Lu³⁺ calculated from XRD patterns was similar to that of YAG single crystal, and its fluorescent intensity arising from ⁴F3/2?→?⁴I9/2 transition of Nd³⁺ ions reached the maximum although the ceramic was opaque. The results indicated that Lu³⁺ ions under 1.5?at.-% relieved strains from lattice distortion and enhanced the fluorescent intensity.     

Optical and luminescent properties of quasi-stoichiometric YAG: Cr3+ ceramics

The impact of minor stoichiometric variations on the microstructure, optical characteristics, and luminescent properties of YAG:Cr ceramics, synthesized from chemically precipitated ceramic powders, was assessed for the first time. Transparent ceramics with over 70% transparency was produced with a nominal yttrium excess ranging from 0.47 to −1 mol.%. The phase composition, microstructure, and luminescent properties of quasi-stoichiometric YAG:Cr ceramics were examined, and the impact of stoichiometric deviations on the crystal lattice parameter and average grain size in ceramics was outlined. An examination of the optical characteristics of the ceramics revealed a specific absorption band in the case of yttrium excess. The effect of stoichiometry deviation on the luminescent properties of YAG:Cr ceramics was investigated. A change in stoichiometry from −1–0.47 mol.% excess yttrium resulted in a broadening of the luminescence R-line and a decrease in the lifetime of the excited state of Cr³⁺ from 1.91 to 1.81 ms.     

Fabrication and properties of multistage gradient doping Yb:YAG laser ceramics

In order to fully pump and smoothen the temperature gradient of the gain medium, multistage gradient doping Yb:YAG laser ceramics were designed. The composite green bodies were fabricated by tape casting, and multistage gradient doping Yb:YAG ceramics with high optical quality were prepared by vacuum sintering and hot isostatic pressing. For samples pre-sintered at 1740°C for 30 h and then HIP-ed at 1700°C for 3 h in argon at 200 MPa, the in-line transmission values at 1100 nm of YAG, 0.6 at.%Yb:YAG, and 1.5 at.%Yb:YAG ceramics were found to be 83.9%, 84.1%, and 83.3%, respectively. Finally, the 940 nm laser diode was used as the pump source to realize the 1030 nm laser output of multistage gradient doping Yb:YAG ceramic slab with a total energy of 3.43 J. The corresponding optical-to-optical conversion and slope efficiencies were 30% and 45%.     

Viscoelastic behaviors and drying kinetics of different aqueous gelcasting systems for large Nd: YAG laser ceramics rods

Large and nondeforming Nd: YAG ceramic prepared by wet forming is of great importance as gain medium to obtain high-power solid-state lasers. However, it is difficult to achieve high-quality laser ceramics due to insufficiency of the in-depth understanding of transformation mechanism of gels viscoelasticity and effective control means during drying process. In this work, the rheological behaviors, viscoelastic characteristics, and mechanical strengths in classical acrylamide (AM) and novel Isobam (PIBM) gelcastings were systematically compared to explore the suitable route for the large-sized 2% Nd: YAG transparent ceramics with high aspect ratio (>10). AM system exhibited a higher complex viscosity (1.82 × 10⁵ Pa s), a shorter gel time (92.9 seconds), and a higher flexural strength (about 24.46 MPa) than PIBM system, and especially its ability to quickly gel was beneficial to the homogeneity of green body. In addition, the order of drying rates of wet gels in four drying media was observed as follows: 55℃ hot air> ethanol> solid desiccant> PEG-11000 and the moisture diffusion coefficients were calculated and simulated to offer the deep consideration of drying kinetics. The “ethanol + 55℃ hot air” was regarded as an effective composite drying method to eliminate defect and to achieve φ8 mm × 160 mm Nd: YAG ceramic with the in-line transmittance of 83% @1064 nm. Therefore, not only the cognition of gel process, but also the defects control strategy is proposed. More importantly, this work greatly promotes the application of wet forming and laser ceramics in high-power lasers.     

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.     

Some optical,magnetic and transport properties of CdMoO4:Nd3+

Single crystal of new cadmium and neodymium molybdate solid solution (Cd_0.958Nd_0.028□_0.014MoO₄, where □ denotes cationic vacancies) has been successfully grown by the Czochralski method. The X-ray diffraction analysis confirmed that this solid solution crystallizes in the scheelite type structure, the Nd³⁺ ions do not show long-range order and they are randomly distributed in the unit cell, substituting the Cd²⁺ ions. As a consequence, the unexpected properties of CdMoO₄:Nd³⁺ are observed such as the energy gap (~1.77 eV) twice smaller than that of the matrix CdMoO₄, a paramagnetic state with the short-range ferromagnetic interactions, behavior related to the electrical conductor with p–n transition along the 〈100〉 axis, the semiconducting behavior with n–p transition along the 〈001〉 axis and the diode-like behavior found to be of Schottky- or Maxwell-Wagner type. Therefore, we predict great potential of this single crystal for technical applications in electronic devices.     

Synthesis and processing of spinel powders for transparent ceramics

Spinel powders have been synthesized by chemical coprecipitation using two different precursors, nitrates and chlorides, and by an oxides mixture route. It has been shown that depending on the precursors used and the synthesis conditions pure spinel nanopowder can be obtained at different temperatures and with different levels of agglomeration. According to TEM results, the chloride route allows obtaining pure and deagglomerated spinel powders after calcination at 800 °C with a submicrometer particle size. Sintered lyophilized powders obtained by a chloride route allow achieving materials with in-line transmittances close to 46% at 540 nm and 83% in the infrared range.     

Fabrication of YAG transparent ceramics by two-step sintering

Yttrium aluminum garnet (YAG) nanopowders with mean particle size of about 50 nm synthesized by a modified co-precipitation method were used to sinter bulk YAG ceramic by two-step sintering method. Full densification was achieved by heating the sample up to 1800 °C followed by holding at 1550 °C for 10 h. Transparent YAG ceramics were obtained by suppressing grain-boundary migration while promoting grain-boundary diffusion during the two-step sintering process. The microstructure of the YAG ceramic is homogeneous without abnormal grain growth and the transmittance of the sintered sample is 43%.     

Solid-state-reaction fabrication and properties of a high-doping Nd:YAG transparent laser ceramic

High-quality neodymium-doped yttrium aluminum garnet (Nd:YAG) transparent ceramic (4.0 mole percent) was fabricated by a solid-state reaction method and vacuum sintering. The microstructure, optical transmittance, spectral properties and laser performance were investigated. The average grain size of the sample is about 10 mm. The transmittance of a 2.8-mm thick sample reaches 79.5% at the laser wavelength of 1064 nm. The highest absorption peak is centered at 807 nm and the absorption coefficient is 13.9 cm⁻¹. The absorption coefficient at the laser wavelength is 0.2 cm⁻¹. The main emission peak is at 1064 nm and the fluorescence lifetime is 102 μs. A laser diode (808 nm) whose maximum output is about 1000 mW was used as a pump source and an endpumped laser experiment was performed. The 1064 nm-CW-laser output was obtained and the threshold is 733 mW. With 998 mW of maximum absorbed pump power, a laser output of 17 mW is obtained with a slope efficiency of 6.1%. __________ Translated from Journal of The Chinese Ceramic Society, 2007, 35(12): 1600–1604 [译自: 硅酸盐学报]     

Heating parameter optimization and optical properties of Nd:YAG transparent ceramics prepared by microwave sintering

Nd-doped YAG transparent ceramics were prepared by microwave sintering. In this paper, the green bodies from high-purity commercial powders were sintered from 900 °C to 1750 °C for different lengths of time (0.5–2 h) by microwave heating. By optimizing the microwave heating parameters (the heating rate at different stages of microwave sintering, sintering temperature and holding time), the microstructures and optical properties of transparent ceramics can be effectively improved. The phase transformation, densification process and optical properties of Nd:YAG transparent ceramics were discussed. The liquid phases strongly absorb microwave radiation and affect the sintering results of samples during microwave sintering. The highest in-line transmittances of Nd:YAG transparent ceramic fabricated at 1750 °C for 2 h were 76.5% at 400 nm and 80.6% at 1064 nm. The fluorescence emission spectra and lifetime depending on different heating conditions were also discussed.     

Mechanical properties of graphene platelet-reinforced alumina ceramic composites

Alumina (Al₂O₃) ceramic composites reinforced with graphene platelets (GPLs) were prepared using Spark Plasma Sintering. The effects of GPLs on the microstructure and mechanical properties of the Al₂O₃ based ceramic composites were investigated. The results show that GPLs are well dispersed in the ceramic matrix. However, overlapping of GPLs and porosity within ceramics are observed. The flexural strength and fracture toughness of the GPL-reinforced Al₂O₃ ceramic composites are significantly higher than that of monolithic Al₂O₃ samples. A 30.75% increase in flexural strength and a 27.20% increase in fracture toughness for the Al₂O₃ceramic composites have been achieved by adding GPLs. The toughening mechanisms, such as pull-out and crack deflection induced by GPLs are observed and discussed.     

Synthesis of high efficiency Zn2SiO4:Mn green phosphors using nano-particles

In this study, Zn₂SiO₄:Mn²⁺ luminescent phosphors were prepared by mixing nano-scale ZnO, SiO₂, and MnO₂ particles at the compositions corresponding to 2ZnO + SiO₂ + X mol% MnO₂ (Zn₂SiO₄–X-MnO₂, 0.02 ≤ X ≤ 0.05). The mixing powders were calcined from 900 °C to 1300 °C in air and in N₂ atmosphere. No matter calcined in air or in N₂ atmosphere, Zn₂SiO₄ was the mainly crystalline phase in particles calcined at 900 °C and was the only phase in particles calcined at 1000 °C and higher. The influences of MnO₂ concentration and calcining atmosphere and temperature on wavelength of luminescence peak and the emission intensity were further intensively investigated. We would show that the calcining atmosphere had no apparent influences on the physical and photoluminescence (PL) characteristics of Zn₂SiO₄:Mn²⁺ phosphors. The MnO₂ content and the calcining temperature were the main reasons to influence the physical and PL characteristics of Zn₂SiO₄:Mn²⁺ phosphors.