Nanoindentation Characterization of Submicro- and Nano-Sized Liquid-Phase-Sintered SiC Ceramics

Submicro- and nano-sized liquid-phase-sintered SiC ceramics were mechanically tested by nanoindentation in the peak load range 5–400 mN. The submicro-sized sample showed a marked indentation size effect which the nano-sized samples did not exhibit. The relevance of indentation depth with respect to the microstructural scale has been outlined. In the investigated grain-size range, the hardness dependence on the grain size could be described by a load-dependent inverse Hall–Petch relation. Young's modulus was less microstructure- and load-dependent. Because of the very fine microstructure, the nano-sized SiC materials gave lower elastic values than the submicro-sized SiC ceramic.     

Agglomeration Control of Nd:YAG Nanoparticles Via Freeze Drying for Transparent Nd:YAG Ceramics

Neodymium-doped yttrium aluminum garnet (Nd:YAG) nanopowders were synthesized by the carbonate coprecipitation method. The effects of freeze drying and conventional oven drying of the precursor on the agglomeration of the Nd:YAG nanopowders were compared. The optical properties of the Nd:YAG nanopowders and the corresponding sintered Nd:YAG transparent ceramics were also investigated. The Nd:YAG nanopowders synthesized from freeze-dried precursor showed better dispersion and narrower particle size distribution compared with the powders synthesized from conventional oven drying. As a result, the Nd:YAG nanopowders synthesized from freeze-dried precursor have good sinterability, and Nd:YAG transparent ceramics were fabricated by vacuum sintering at 1750°C for 5 h.     

基于能量平衡方法的压痕尺寸效应分析

针对硬度测试中出现的压痕尺寸效应现象,采用纳米压痕技术与原子力显微技术相结合,得到压痕过程中的载荷与压深加载卸载曲线和压痕三维图,从中可以得到压痕过程中压头所做的塑性功、最大压深、塑性变形面积、塑性变形体积等,并以此为变量提出了一个基于能量平衡方法的改进模型,此模型能更好地解释压痕尺寸效应.单晶硅实验结果表明:在较大压深下,由于形成新表面所消耗的功是出现压痕尺寸效应的主要因素;随着压痕深度的减小,用于克服材料对压头的阻力而消耗的功所起的作用越来越大;而在更小的压深下,用于产生塑性变形的初始能量和测试系统误差所造成的影响会越来越大,不可忽视.     

Microstructural Evolution During Vacuum Sintering of Yttrium Aluminum Garnet Transparent Ceramics: Toward the Origin of Residual Porosity Affecting the Transparency

Controlling residual amount of defects in transparent ceramics is a major challenge for laser applications. This study was focused on microstructural evolution of Nd:YAG ceramics during their reactive solid‐state sintering which was correlated to their optical transmittance. From microstructural observations, the microstructural maps and grain size‐density and grain size‐pore size sintering trajectories of Nd:YAG ceramics were established as a function of silica content. For densities higher than 99.7%, the occurrence of intragranular porosity was correlated to a critical pore radius of 0.16 μm. Silica appears to favor the formation of intragranular porosity which was attributed to the increasing of the grain growth rate compared with the densification one. An analytical model was established by coupling the analytical laws derived from sintering trajectories and the classical theory of light diffusion, allowing to correlate the microstructural features of transparent Nd:YAG ceramics to their optical properties.     

YAG纳米粉体的制备技术研究进展

近年来YAG纳米粉体因其具有特殊的性能而备受人们的关注。以此为原料采用先进的陶瓷制备工艺可以得到透明的YAG固体激光工作介质 ,其物理化学及光学性能可与单晶相比拟。YAG粉体通过掺杂Ce3 ,Tb3 ,Eu3 等离子还可以作为超短余辉荧光粉 ,在发光材料领域有广泛的应用。本文着重介绍了目前应用较多的几种YAG纳米粉体的制备方法 ,并简要地比较了各种方法的优劣。     

Residual porosity and optical properties of spark plasma sintered transparent polycrystalline cerium-doped YAG

Transparent cerium-doped yttrium aluminum garnet (Ce:YAG) phosphors are promising candidates for high-power white light emitting diode applications. In the present study, Ce:YAG powder was synthesized by a co-precipitation method and highly transparent ceramics were fabricated by spark plasma sintering. The effects of temperature and pressure, as well as post-sintering treatments (annealing or hot isostatic pressing), on residual porosity were studied by electron and confocal laser microscopy. Correlation between residual porosity characteristics (pore size and volume fraction) and optical properties (in-line transmittance and photoluminescence intensity) of the luminescent transparent ceramics was established.     

Cracking and the Indentation Size Effect for Knoop Hardness of Glasses

The Knoop hardnesses of five glasses decreased with increasing load in accordance with the classic indentation size effect (ISE). At moderate loads, cracking dramatically altered the indentation sizes and the ISE trends in three of the five glasses. Cracked indentations were as much as 10 μm longer than uncracked indentations made under identical conditions. Diagonal length readings must be corrected for optical resolution limitations if low power lenses are used.     

黏弹材料动态纳米压入过程的尺度效应

提出柔度因子分析法表征压入尺寸效应（ISE)通讨聚甲基丙烯酸甲酯(PMMA)及热塑性聚氨酯(TPU)的动态纳米压痕试验,探讨黏弹材料动态压入过程中的压入尺度效应及其影响因素。结果表明,Berkovich针尖对黏弹材料进行纳米压痕动态测试时,主载荷是压入尺度效应产生与否的决定因素,频率对此影响较小,谐振载荷控制方式影响甚微;测试材料存在一临界值,当压入深度大于其临界值时,动态纳米压痕测试获得的黏弹材料参数与传统的动态力学分析(DMA)试验结果基本一致。     

钇铝石榴石(YAG)激光透明陶瓷研究进展

钇铝石榴石(YAG)激光透明陶瓷由于具有单晶、玻璃激光材料无可比拟的优势而成为研究热点,并得到迅速发展,高性能的稀土元素掺杂YAG透明激光陶瓷被相继报导.本文综述了近年来国内外关于YAG激光透明陶瓷的最新研究成果.主要包括YAG微细粉体合成、烧结添加刺及多晶YAG透明陶瓷的致密化烧结技术,并对比了YAG透明陶瓷相对于Y...     

Yb3+掺杂YAG微晶玻璃的制备与晶化性能研究

通过对CaO-Al2O3-SiO2三元相图相关点的探讨,确定Yb3+掺杂的29.5SiO2-30.5CaO-24 Al2O3-12Y2O3-4 Yb2O3-(0～3)ZrO2玻璃系统,采取高温熔融获得母体玻璃。用DTA和梯温法测定母体玻璃的析晶行为并确定热处理制度。采取XRD,TEM分析热处理后的样品。结果表明,选择的玻璃成分均可得到Yb3+掺杂YAG透明微晶玻璃,含3 mol%ZrO2更有利于得到晶体颗粒的形貌和大小基本一致、分散均匀、尺寸约33 nm的Yb3+掺杂YAG透明微晶玻璃。     

钇铝石榴石透明激光陶瓷的研究进展

透明钇铝石榴石(aluminum-yttrium garnet,YAG)陶瓷具有良好的化学稳定性和光学性能,是一种很有前途的单晶激光材料的替代物。同单晶相比,多晶YAG陶瓷具有许多优点,如：大尺寸材料易于制备,成本低适合大规模生产等。此外,因掺杂浓度高可得到较大的输出功率。对透明YAG激光陶瓷的光学特性以及制备工艺做了重点介绍,并对研究进展进行综合评述。最后,展望该领域的发展前景及今后的研究趋势。     

Optical properties of YMASG:Ce fluorescent ceramics prepared by hot-pressure sintering

Cerium-doped yttrium aluminum garnet (YAG:Ce) based transparent ceramics have been widely used in fluorescent lighting as high-quality inorganic fluorescent conversion materials. This paper further explores the Mg²⁺-Si⁴⁺ ions doped YAG:Ce transparent ceramics by combining the solid-phase reaction method with vacuum hot-pressure sintering and implementing protection measures against hot-pressure mold contamination, and also investigates the effect of different Mg²⁺-Si⁴⁺ doping contents on the structure, transmittance and luminescence properties of the ceramics under hot-pressure sintering. In this work, pure-phase YMASG:Ce transparent fluorescent ceramics with a grain size of about 3-6 μm and clear and clean grain boundaries were obtained with an In-line transmittance of 67% at 800 nm. Under the excitation at 460 nm, the emission peak was red-shifted by 26 nm and the full width at half maxima (FWHM) was broadened with the increase of Mg²⁺-Si⁴⁺ content, which shows that the Mg²⁺-Si⁴⁺ ion pair effectively complements the absence of the red light component in the YAG:Ce emission spectrum. The optimized YMASG:Ce ceramics obtained high-quality warm white light with a low correlated color temperature (CCT) and a high color rendering index (CRI) under the excitation of the blue LED chip. This work proved the feasibility of vacuum hot-pressure sintering to prepare YMASG:Ce transparent fluorescent ceramics, and provided a new approach for studying YMASG:Ce-based ceramics, which was significant for the application of high-power visible laser illumination.     

Fabrication and properties of transparent Tb:YAG fluorescent ceramics with different doping concentrations

Terbium doped yttrium aluminum garnet (Tb:YAG) transparent ceramics with different doping concentrations were fabricated by the solid-state reaction method using commercial Y₂O₃, α-Al₂O₃ and Tb₄O₇ powders as raw materials. Samples sintered at 1750 °C for 20 h were utilized to observe the optical transmittance, microstructure and fluorescence characteristics. It is found that all the Tb: YAG ceramics with different doping concentrations exhibit homogeneous structures with grain size distributions around 22–29 µm. For the 5 at% Tb:YAG transparent ceramics, the grain boundaries are clean with no secondary phases. The photoluminescence spectra show that Tb:YAG ceramics emit predominantly at 544 nm originated from the energy levels transition of ⁵D₄→⁷F₅ of Tb³⁺ ions, and the intensity of the emission peak reaches a maximum value when the Tb³⁺ concentration is 5 at%. The in-line transmittance of the 5 at% Tb:YAG ceramics is 73.4% at the wavelength of 544 nm, which needs to be further enhanced by optimizing the fabrication process. We think that Tb:YAG transparent ceramics may have potential applications in the high-power white LEDs.     

Sintering additives regulated Cr ion charge state in Cr doped YAG transparent ceramics

Cr: YAG and Cr, Nd: YAG transparent ceramics have significant application prospects in solid state lasers, therefore a controllable charge state of Cr ion in Cr doped YAG transparent ceramics is necessary. In this study, a successful regulation of Cr charge state in both Cr, Nd: YAG and Cr: YAG transparent ceramics was achieved, by a simple optimizing the sintering additives. Both ceramics with the Cr doping concentration of 0.3?at% reached to the theoretical transmittance, after the vacuum sintering and the subsequent annealing process. It was found that by adopting silica additive, divalent charged Cr²⁺ ions could be detected from the vacuum sintered samples, and they were transferred into trivalent state after further annealing in air. Meanwhile, by vacuum sintering ceramics with divalent additives (CaO and MgO), a stable trivalent charged Cr ion could be obtained, and the subsequent air annealing process indicated a significant conversion from Cr³⁺ to Cr⁴⁺. Further increasing the Cr concentration was not benefit to the optical quality as well as the conversion of Cr³⁺ ion in Cr, Nd: YAG transparent ceramics.     

Single CaO accelerated densification and microstructure control of highly transparent YAG ceramic

In this work, a small amount of CaO single dopant was adopted to realize the densification and microstructure control of fine grained YAG ceramic with excellent optical quality, by a simple solid‐state reaction and one‐step vacuum sintering method. Then, highly transparent YAG ceramics (T = 84.4% at 1064 nm) were obtained just after vacuum sintering at 1820°C for 8 hours. The average grain size was only 2.7 μm, when the total amount of CaO was as low as 0.045 wt%. The effect of CaO on the microstructural evolution and optical property of the as‐fabricated YAG ceramics was systematically investigated in detail. It was found that CaO dopant promoted both densification and grain growth of YAG ceramics when the sintering temperature was lower than 1660°C, however, it dramatically inhibited grain growth when the sintering temperature was further increased.     

Upconversion luminescence of high content Er-doped YAG transparent ceramics

The various high content Er-doped YAG transparent ceramics with excellent transparency up to nearly 84% at the visible band and the near-infrared band were prepared by the solid-state reaction and the vacuum sintering technique. It is found that the samples exhibit pore-free structures and there are no secondary phases both at the grain boundaries and the inner grains. The average grain size of the Er:YAG ceramics is about 30 μm. The green and red upconversion luminescences in the Er:YAG ceramics pumped by a 980 nm LD were observed. The different upconversion mechanisms depending on Er content in the Er:YAG ceramics and the LD power were also discussed.     

Knoop Microhardness Anisotropy and the Indentation Size Effect on the Basal Plane of Single-Crystal Alumina (Sapphire)

The Knoop microhardness anisotropy profile was determined for the basal plane of a Czochralski grown alumina single crystal for indentation test loads from 100 through 1000 g. Microhardness maxima occur at low indentation test loads for the long axis of the Knoop indenter parallel to the 〈2[Onemacr][Onemacr]0〉. Minima exist for the long axis parallel to the 〈10[Onemacr]0〉. This low indentation test load profile is attributed to slip on the primary slip system, the (0001)〈[Onemacr][Onemacr]20〉, as previously noted by Brookes and co-workers. The degree of the microhardness anisotropy decreases for higher indentation test loads. This results from the activation of multiple slip systems to accommodate the greater amounts of plastic flow required by the larger indentation sizes. The microhardness profile becomes more uniform with increasing indentation test load until the Knoop microhardness approaches a test-load-independent, orientation-independent microhardness of 1167 ± 34 kg/mm². The indentation size effect (ISE) was further investigated through lubricated indentation hardness measurements. Lubrication of the test specimen surface significantly reduces the ISE. Results indicate that friction between the test specimen surface and the indenter facets is a major portion of the ISE.     

Effect of Load on the Hardness of Hot Isostatically Pressed Silicon Nitride

The hardness values of five hot isostatic pressed silicon nitride materials, with varying densities, were measured at loads between 1 and 200 N. For the fully dense materials, the calculated hardness decreased from about 30 to 15 GPa as the load increased to about 10 N, and the hardness remained constant at higher loads. For the samples that showed indentation size effect (ISE), cracks formed at the corners of the indentation, starting at the lowest load of 1 N. Materials with lower densities had lower hardness values, displayed a very small or no ISE, and formed corner cracks only at high loads. For the samples that displayed an ISE at low loads, the formation of cracks was analyzed using the Niihara et al . criterion for Palmqvist cracks.     

Fabrication and Optical Properties of Highly Transparent Er:YAG Polycrystalline Ceramics for Eye‐Safe Solid‐State Lasers“

Highly transparent 1 at.% Er:YAG ceramics was fabricated by a reactive sintering method under vacuum. The optical properties, the microstructure and the laser performance of the Er:YAG ceramics were investigated. The average grain size of the Er:YAG ceramics was 7~8 μm. The in‐line transmittances of the Er:YAG ceramics at the wavelength of 1800 and 400 nm were about 84.6% and 82.4%, respectively. The absorption coefficient of the Er:YAG ceramics was 1.29 cm^?1. The grain boundaries were very clean and no secondary phase was observed. When end‐pumped by an Er,Yb‐fiber laser at 1532 nm, a maximum output power of 13.8 W lasing at the wavelength of 1645 nm was obtained with a slope efficiency of 54.5%.     

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.