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.     

Influence of high energy ball milling on structural,microstructural and optical properties of TiO2 nanoparticles

The influence of high-energy ball milling on structural, microstructural, and optical properties of TiO₂ by modifying the nanoparticle size was studied. Five samples were extracted at different milling times (0, 2, 4, 8, and 13 h). The average particle sizes estimated by dynamic light scattering (DLS) were 205, 155.8, 116.8, 82.9, and 82.7 nm at 0, 2, 4, 8, and 13 h, respectively. X-ray diffraction analysis confirmed progressive broadening of the peaks as the milling time elapsed. Besides, a correlation was found between d spacing and the average crystal size. The UV–Vis diffuse reflectance spectra of TiO₂ revealed a decrease in reflectance due to particle size reduction. Similarly, an alteration of the bandgap transition energy was presented, whose values gradually decreased from 2.966 eV to 2.861 eV for the sample without and with the maximum duration milling performed (13 h), respectively. Likewise, the SEM analysis showed a distribution in nanoparticle size that became more homogeneous and smaller average grain size as the milling duration was longer.     

Effect of SiC nanoparticle content and milling time on the microstructural characteristics and properties of Mg-SiC nanocomposites synthesized with powder metallurgy incorporating high-energy ball milling

The fabrication of magnesium nanocomposites with a homogeneous dispersion of nanoparticles has recently become an important issue. In the current study, micro-sized magnesium powders reinforced with 10, 20, and 30 wt% SiC nanoparticles were synthesized through high-energy ball milling using milling times ranging from 1 to 20 h to overcome the segregation and agglomeration of nanoparticles within the magnesium matrix. The milled nanocomposite powders were then consolidated using uniaxial cold pressing and sintering processes. Scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and X-ray diffraction were employed to investigate the effects of different milling times and contents of SiC nanoparticles on the evolution of the morphology of Mg–SiC milled powders and the microstructural characteristics of Mg–SiC sintered samples. In addition, once the consolidation process was complete, the relative densities and hardness values of the Mg–SiC nanocomposites were examined. The results indicated that as the content of SiC nanoparticles and the milling time increased, finer and equiaxed nanocomposite powders were obtained, and the average crystallite size of the milled magnesium powder significantly decreased. A homogeneous distribution of the SiC nanoparticles, including up to 30% of weight fraction, in the magnesium matrix was confirmed after 20 h of milling by elemental mapping generated by EDS. Additionally, the XRD analysis revealed that the diffraction peaks of the magnesium broadened while their maximum intensities decreased with increasing the milling time and SiC content. No undesirable phases were formed by interfacial reactions between magnesium and SiC nanoparticles in the milled nanocomposite powder during mechanical alloying. Furthermore, the results showed that both the relative density and hardness value of the Mg–SiC sintered sample improved as the milling time increased. However, the relative density of the Mg–SiC nanocomposite drastically decreased while the hardness significantly improved, as a result of increasing the content of SiC nanoparticles.     

Effect of MgO doping on the structure and optical properties of YAG transparent ceramics

The paper studies the features of Mg²⁺ ions as sintering aid for reactive solid-state sintering of YAG transparent ceramics. Phase composition, microstructure and optical properties of YAG ceramics, doped by 0 ÷ 0.15 wt.% MgO, were investigated. Solubility limit of Mg²⁺ ions in YAG crystal lattice was found to be in the range of 0.06 ÷ 0.1 wt.% of MgO additive. Substitution mechanism of Mg²⁺ in ceramic YAG was identified by comparison of XRD data and ab initio calculation. It was shown that within the solubility limit Mg²⁺ ions most likely substitute Al³⁺ sites. Doping by MgO above solubility limit led to precipitation of spinel secondary phases. It was found that doping by Mg²⁺ ions increases concentration of oxygen vacancies in YAG lattice that effectively promote sintering. The optimal concentration range of MgO sintering aid that allow to achieve YAG transparent ceramics was defined as 0.03 ÷ 0.06 wt.%.     

球磨时间对石墨烯复合材料电化学性能的影响

采用X射线衍射仪（XRD）、扫描电子显微镜（SEM）和电化学工作站等手段研究了球磨时间（0~60 min）对石墨烯/La₁₅Fe₂Ni₇₁Mn₆B₂Al₂复合材料微观结构和电化学性能的影响。结果表明,球磨时间为0~60 min制备的石墨烯复合储氢合金都主要由La₃Ni₁₃B₂、（Fe,Ni）、LaNi₅相组成,其中LaNi₅相的晶胞体积会随着球磨时间的增加而减小。随着球磨时间从0 min增加至60 min,石墨烯复合储氢合金的电荷转移电阻先减小后增大、交换电流密度先增大后减小、氢扩散系数和荷电保持率先增加后减小,在球磨时间为40 min时取得电荷转移电阻最小值,交换电流密度、氢扩散系数和荷电保持率最大值。此外,在相同循环次数下球磨时间为40 min制备的石墨烯复合储氢合金具有相对较高的放电比容量。适宜的石墨烯/La₁₅Fe₂Ni₇₁Mn₆B₂Al₂复合材料的球磨时间为40 min,此时氢扩散系数和荷电保持率分别为1.259×10^-8 cm²/s和97.62%,具有较好的电化学性能,这主要与此时复合材料粉末颗粒较为细小、均匀且结晶度较高等有关。     

The effect of high-energy ball milling on the electromechanical strain properties of Bi-based lead-free relaxor matrix ferroelectric composite ceramics

The crystal structure, ferroelectric, and electric-field-induced strain (EFIS) properties of Bi-based lead-free ferroelectric/relaxor composite materials are investigated. Bi_1/2(Na_0.82K_0.18)_1/2TiO₃ as a ferroelectric material and 0.98Bi_1/2(Na_0.78K_0.22)_1/2TiO₃‒0.02LaFeO₃ as a relaxor were synthesized via conventional ceramic processing routes while the relaxor (matrix phase) was prepared via high-energy ball milling (HEBM) after calcination. The average particle size was decreased via HEBM treatment. As a result, a high d₃₃^* value of over 600 pm/V was obtained at 4 kV/mm for 30-min HEBM-treated composites. This demonstrates that HEBM treatment is effective in enhancing the strain properties of lead‒free piezoelectric composite materials.     

MgO assisted densification of highly transparent YAG ceramics and their microstructural evolution

In current study, various amounts of MgO single dopant was adopted to fabricated high quality transparent YAG ceramics, by utilizing a simple one-step solid state reaction sintering method in vacuum. At a MgO doping amount of only 0.03 wt.%, YAG transparent ceramics with a transmittance of 84.5% at 1064 nm could be obtained, after sintering at 1820 °C for 8 h. The microstructure evolution and optical property of as-fabricated YAG ceramics as a function of MgO doping concentration were systematically investigated. MgO dopant could effectively promote densification of YAG ceramics when the sintering temperature was lower than 1660 °C, and dramatically accelerate its grain growth between 1540 °C and 1660 °C. Further increase the doping amount of MgO would not benefit to the optical quality of YAG ceramics, and the intragranular pores as well as the Mg-riched secondary phase were observed from the MgO heavily doped ceramics.     

Preparation and optical properties of dispersible ZnSe nanocrystals synthesized by high energy ball milling

ZnSe nanocrystals have been successfully synthesized by high energy ball milling method. X-ray diffraction patterns show a single zinc blende structure formed in the milling process. HRTEM images confirm that the formation of the ZnSe nanocrystals synthesized by high energy ball milling have a wide crystals distribution (3–20 nm). Using the aqueous solutions of Na₃PO₄, (NaPO₃)₆ and Na₄P₂O₇ to disperse the 40 h-milled samples, we have observed the gradual blue-shift of the absorption edge along with the different centrifuging speed. In PL spectras, two main bands peaked at about 1.95 and 2.35 eV are observed, the former band is related to the V_Zn defects emission; and the latter is related to the V_Se defects emission. The V_Se defects emission does not depend on the dispersants, but the V_Zn defects emission changes in different dispersants.     

Effect of milling ball size on the densification and optical properties of transparent Y2O3 ceramics

In this study, we report highly transparent Y₂O₃ ceramics fabricated by hot-pressing only at 1500 °C without a HIP treatment, featuring in-line transmittance levels of 77% and 84% at a wavelength of 400 and 1100 nm, respectively with the grain size suppressed to 710 nm. The effect of the ball size during the grinding of Y₂O₃ powders on the correlation between the thus-prepared Y₂O₃ powders and the optical properties of the hot-pressed samples is demonstrated for the first time. With a decrease in the diameter of the ZrO₂ balls from 5 mm to 1 mm, the milling efficiency was enhanced and admirable transparency of Y₂O₃ was attained at a short milling time. However, several micron-sized pores remained in the transparent specimens prepared with 1 mm balls, originating from the inhomogeneously packed region of the green body. Finally, the 2 mm was found to be optimum for obtaining a fine-grained and pore-free microstructure with the best in-line transmittance of Y₂O₃ ceramics.     

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.     

Influence of ball milling contamination on properties of sintered AlN substrates

The AlN substrate was fabricated by the tape casting process, and its thermal conductivity and electrical conductivity were investigated for various ball milling times and types of milling media. The oxygen content was measured after ball milling, de-binding process, and sintering. The oxygen content after the de-binding process was 1.2–2.3 wt%, similar to that after milling. After the de-binding process, the specimens were sintered at 1850 ℃ for 3 h in nitrogen atmosphere. The thermal conductivity of the sintered specimens decreased from 158 W m⁻¹ K⁻¹ to 100 W m⁻¹K⁻¹ with increasing milling time. Simultaneously, the electrical conductivity decreased from approximately 10⁻⁷ Ω⁻¹ cm⁻¹ to 10⁻⁹ Ω⁻¹ cm⁻¹ at 500 °C when Al₂O₃ or ZrO₂ balls were used, whereas the electrical conductivity did not decrease when Si₃N₄ balls were used.     

Transparent ceramics green-microstructure optimization by pressure slip-casting: Cases of YAG and MgAl2O4

This paper presents experimental data and its interpretation regarding the forming of YAG and spinel green-bodies, intended for transparent parts fabrication, by the pressure slip casting (PSC) method. Conditions for an optimal operation are established based on the modeling of the filtration kinetics. It emerges that the method is able to provide highly sinterable green parts by ensuring that the cakes porosity exhibits low average size and narrow size distribution. Results were compared with other popular forming approaches like slip casting (SC) and cold isostatic pressing (CIP). PSC was found as superior, to the other approaches, as far as obtainment of high sinterability green- bodies is concerned. In the case of YAG, it was shown that PSC method even allows the replacement of the traditional long vacuum firings by a two stage densification operation in which an initial air-firing is completed by a hot isostatic pressing step.     

Influence of powder physicochemical characteristics on microstructural and optical aspects of YAG and Er:YAG ceramics obtained by SPS

The present work aims to establish a correlation between the characteristics of YAG and Er:YAG commercial powders produced by two different synthesis routes and sintered ceramic microstructures and their optical aspect by taking into account the influence of pressure applied during the Spark Plasma Sintering (SPS) process. Physical and chemical characteristics of the powders were compared using various techniques such as SEM, XRD, laser diffraction and chemical analyses. Their behaviours were evaluated through a rheological study, compressibility tests and dilatometry cycles using SPS. This paper pinpoints the most important powder features which influence the optical quality of YAG and Er:YAG ceramics. The optical quality is mainly affected by the porosity, related to powder characteristics that affect particle rearrangement, densification and grain growth. The applied pressure induces microstructural heterogeneities depending on the starting material used and resulting in core-shell aspects of sintered ceramics.     

高能球磨作用对合成堇青石基陶瓷的相组成和相变机理的影响

采用XRD分析研究了由分析纯的氧化物粉末制备堇青石基陶瓷时,高能球磨作用及热处理温度对堇青石陶瓷相组成和相变过程的影响,并分析了高能球磨在堇青石陶瓷烧成过程中的作用.结果表明经高能球磨处理的试样在低温烧成(900℃)时,首先出现中间相镁铝尖晶石(MgAl2O4),但1100℃时中间相又消失;与未球磨的试样比较,高能球磨不仅能够降低堇青石的相变温度,而且可大大加快中间相和原料相向α-堇青石转变的速度;同时发现提高烧成温度有利于中间相向堇青石的转变.此外,还研究了粉末的状态(即是否经成型处理)对堇青石陶瓷相组成的影响.结果表明,加压成型使Si4+、Mg2+和Al3+易于扩散,能促进早期的固相烧结和后期的液相烧结,有利于主晶相α-堇青石的合成,但对相组成没有太大影响.     

Effect of rare earth ions doping on the thermal properties of YAG transparent ceramics

Yttrium aluminium garnet doped with rare earth ions is one of the most common active media in solid state lasers. In high-power lasers, thermal management is crucial, requiring information on the thermal properties. In this work, the thermal diffusivity and conductivity of polycrystalline YAG ceramics doped with Yb and Er were measured by laser flash method at various temperatures ranging from room temperature to 900 °C. Transparent ceramic YAG samples were prepared by solid state reactive sintering of oxide powders under vacuum. Thermal diffusivity and conductivity showed similar trends, decreasing with increasing temperature as well as with the increase of dopant content from 0 to 20 at.%. The measured values were compared with literature data and empirical relations. Similar values were obtained both for Yb and Er doping. We thus suggest that the data of thermal diffusivity and conductivity of Yb:YAG may be used as a first approximation for Er:YAG.     

Microstructure and mechanical properties of fine-grained boron carbide ceramics fabricated by high-pressure hot pressing combined with high-energy ball milling

Dense and fine-grained boron carbide (B₄C) ceramics were fabricated via high-pressure hot pressing (100?MPa) using powders, which are prepared by high-energy ball milling. These powders were sintered at a low temperature (1800?°C) without any sintering aid. The dense and fine-grained B₄C ceramics demonstrate super high hardness, outstanding fracture toughness and modern flexure strength. The milled powders were characterised by disordered crystal structure and ultrafine particle size that ranges from a few nanometres to a few hundred nanometres. The combined contributions of high pressure and the characteristic of the milled powders guaranteed that the dense fine-grained microstructure was achieved at only 1800?°C. The grain size distribution of the ceramics was inhomogeneous and ranged from 70?nm to 1.6?µm. However, the average grain size was fine at only 430?nm, which partially contributed to the super high hardness of the B₄C ceramics. The locally concentrated areas of the small grains changed the fracture mode of the B₄C ceramics from the complete transgranular fracture to a mixture of transgranular and intergranular fractures, thereby enhancing the toughness of the B₄C ceramics. The relative density, Vickers hardness, flexure strength and fracture toughness of the obtained B₄C ceramics reached up to 99.5%, 41.3?GPa, 564?MPa and 4.41?MPa?m^1/2, respectively.     

Co-precipitation synthesis and two-step sintering of YAG powders for transparent ceramics

Yttrium aluminum garnet (Y₃Al₅O₁₂, YAG) precursor was synthesized by the co-precipitation method with ammonium hydrogen carbonate as the precipitant. The influence of aging and calcination temperature on the precursor composition and transformation temperature of the YAG phase was investigated. On that basis, a two-step sintering (TSS) method (heating the sample up to 1800 °C followed by holding it at 1600 °C for 8 h) was used to fabricate bulk transparent YAG ceramics in vacuum (10⁻³ Pa) in this communication. A variety of techniques, such as X-ray powder diffraction, infrared spectra, scanning electron microscopy and UV–vis–NIR spectrophotometry were adopted to characterize the resulting YAG powders and ceramics. The results showed that aging had a dramatic effect on the precursor composition, which in turn influenced the transformation temperature of the YAG phase. Loosely agglomerated YAG powders with a mean particle size of 50 nm were obtained by calcinating the precursor without aging at 1000 °C. Finally, a transparent YAG ceramic specimen, achieving the in-line transmittance of 41% in the visible wavelength region and a nearly pore-free microstructure with uniform grains of about 4 μm, was produced via the TSS technique.     

Quantitative relationship between microstructure and mechanical properties in Nd: YAG transparent ceramics

In this work, stereology and fractals were applied to identify the quantitative relation between stereology parameters, fractal dimension, and mechanical properties of Nd: YAG transparent ceramics sintered at 1750 °C for 8–50 h. Mechanical properties and microstructure of the samples were investigated by using universal testing machine, micro-hardness tester, and scanning electron microscopy (SEM), respectively. When the ceramics were sintered at 1750 °C for 50 h, the compressive strength, flexural strength, and Vickers hardness reached 381.6 ± 5.2 MPa, 275.0 ± 5.5 MPa, and 1330.4 ± 18.5 MPa, respectively. Besides, the fracture toughness of ceramic samples was calculated by Vickers hardness. Micrographs of the sample surface and frequency distribution of crystal grains were analyzed by using metallographic image analyzer software. Findings suggest that compressive strength, flexural strength, and Vickers hardness linearly increase upon an increase in equivalent sphere diameter (D_3S). However, compressive strength, flexural strength, and Vickers hardness decrease as a function of specific surface area per unit volume of the grains (S_V) and discrete grains (S_VP) and mean free distance (λ). Perimeter and area of crystal grains were obtained by using Image-Pro Plus image analysis software. The relationship between the fractal dimension of grain boundary and mechanical properties was analyzed based on the area-perimeter (small-island) method. When the grain boundary fractal dimension is close to 1.0, the geometry of ceramic grains tends to be regular, and mechanical properties of ceramic samples increases.     

Effect of high-energy ball milling on the microstructure and properties of ultrafine gradient cemented carbides

Planetary low-temperature high-energy ball mill was used for preparing the mixed powders with different particle sizes by adjusting the milling time. The ultrafine grain gradient cemented carbides were prepared by sinter-HIP treatment. The effects of milling time on the gradient formation, grain growth, and mechanical properties of ultrafine grain gradient cemented carbides were investigated. The results show that the high-energy ball milling cannot effectively reduce the particle size of mixed powder with short milling time. In addition, the particle size of the mixed powder is significantly reduced, while the specific surface area is significantly increased when the ball milling time exceeds 25 hours. The gradient layer thickness and the grain size increase at the beginning and then decrease when the mixed powder particle size was decreased. Simultaneously, the density, hardness, and fracture toughness of the alloy increase gradually. On the contrary, the number of WC with abnormal grain growth is significantly increased. The thickness of the gradient layer reached 32 μm, and the mean WC grain size is 314 nm. Based on the analyzed results, an optimized gradient layer thickness, grain size, density, and hardness can be obtained when the ball milling time is 35 hours.     

Isobam assisted slurry optimization and gelcasting of transparent YAG ceramics

Gelcasting is a simple near-net shaping method to fabricate large-sized and/or complicated-structural ceramics. In this paper, a transparent yttrium alumina garnet (YAG) ceramic was successfully fabricated by gelcasting with a nontoxic, water soluble copolymer (isobutylene and maleic anhydride, Isobam) as both dispersant and gelling agent. The rheological behaviors of the slurries with different solids loading and Isobam contents were systematically investigated. The optimized slurry of 0.5 wt% Isobam and the solid loading of 68 wt% had the low viscosity and high stability, resulting in better homogeneity of the green body and better optical quality of transparent ceramics. A nearly pore-free structure of the sintered YAG ceramics with average grain size about 10.0 µm was obtained possessing an in-line transmittance of 75.7% at the wavelength of 1064 nm for a sample 2.5 mm thick.