Effect of heat treatment on green machinability of SiAlON compacts

SiAlON based ceramics are promising materials for wear applications such as wire extrusion dies, pipe bending rollers, etc. due to their outstanding mechanical properties both at high and low temperatures. To be able to utilize these materials for such applications, they should have specific geometrical details as holes, threads, groves, etc. for the ease of fixation. Machining of a ceramic component in its green state is one of the most common techniques which enable producing SiAlON wear parts with desired geometries. It is a prerequisite for green machining that the compact should have a sufficient green strength to withstand against stresses at the cutting zone during machining. In this study, the required green strength was obtained by a simple heat treatment step performed between 1100 and 1400 °C. The effect of this process on the microstructure, phase development, strength and machinability of SiAlON green compacts were investigated. It was observed that the compacts heat treated at 1400 °C provide a sufficient strength against damage formation on the machined part and a relatively low tool wear as a result of the formation of fragmented chips during the cutting process. Although these fragmented chips have beneficial effects on the tool wear, they resulted in a relatively poor surface quality in the machined parts.     

SiAlON材料的氧化行为

SiAlON材料在高温氧化气氛下的氧化行为和氧化机理一直是材料科学领域关注的焦点.本文综述了SiAlON材料氧化的相关研究,分析对比了单相和复相SiAlON材料的氧化行为,讨论了SiAlON材料的氧化影响因素以及氧化机理,指出了SiAlON材料氧化研究存在的问题.     

Molecular-level composition design for efficient synthesis of SiAlON ceramics

SiAlONs are a class of liquid-phase sintered ceramics with excellent room-temperature strength and toughness, but whose residual grain boundary glass softens at high temperatures, limiting use in extreme environments. For this reason, efforts are made to minimize the volume of the grain boundary glass while still facilitating full densification. This work describes a potential route for the densification of SiAlONs with very low concentrations of liquid-phase sintering additive (e.g., rare-earth oxides such as yttria) by using an organometallic precursor. Solid solution of Al and O in the Si₃N₄ lattice was accomplished through the incorporation of solute atoms via liquid organic precursor aluminum sec-butoxide (ASB). Al₂O₃ powder is conventionally used for this purpose, and the subsequent lattice softening associated with the solid solution helps to facilitate densification. However, a liquid-phase additive is still essential for the full densification of SiAlONs. Higher densities were obtained from SiAlON powder blends utilizing organometallic ASB than those utilizing alumina powder, allowing for greater densification at very low Y₂O₃ concentrations. The thermal decomposition of the organic precursor was investigated by high-temperature scanning electron microscopy, thermogravimetric analysis, and various X-ray diffraction experiments. Immersion density measurements and lattice parameter refinements were performed for samples sintered with varying Y₂O₃ concentrations and/or dwell times. Results indicate that ASB-containing powder blends favor SiAlON formation more strongly than Al₂O₃-containing powder blends and favor densification at very low Y₂O₃ concentration.     

Green emitting β$\ubeta$-SiAlON:Eu2+ phosphors derived from chemically modified perhydropolysilazanes

We report the first synthesis of β-SiAlON:Eu²⁺ phosphors from single-source precursors, perhydropolysilazane (PHPS), chemically modified with Al(OCH(CH₃)₂)₃, and EuCl₂. The reactions occurring during the precursor synthesis and the subsequent thermal conversion of polymeric precursors into β-SiAlON:Eu²⁺ phosphors have been studied by a complementary set of analytical techniques, including infrared spectroscopy, gas chromatography–mass spectrometry, thermogravimetry–mass spectrometry, X-ray diffraction (XRD), photoluminescence spectroscopy, and scanning electron microscopy. It has been clearly established that Al(OCH(CH₃)₂)₃ immediately reacted with PHPS to afford N–Al bonds at room temperature, whereas N–Eu bond formation was suggested to proceed above 600°C accompanied by the elimination of HCl up to 1000°C in flowing N₂. The subsequent 1800°C-heat treatment for 1 h under an N₂ gas pressure at 980 kPa allowed converting the single-source precursors into fine-grained β-SiAlON:Eu²⁺ phosphors. XRD analysis revealed that the Al/Si of .09 was the critical atomic ratio in the precursor synthesis to afford single-phase β-SiAlON (z = .55). Moreover, Eu²⁺-doping was found to efficiently reduce the carbon impurity in the host β-SiAlON. The polymer-derived β-SiAlON:Eu²⁺ phosphors exhibited green emission under excitation at 460 nm and achieved the highest green emission intensity at the critical dopant Eu²⁺ concentration at 1.48 at%.     

用于白光LED稀土Eu掺杂SiAlON基荧光粉的发光性能

SiAlON基荧光粉因其优异的化学和物理稳定性,成为近年来发光领域的一个研究热点,尤其在LED等领域,受到研究者的热切关注。稀土掺杂SiAlON基荧光粉体有望成为新一代照明光源。由于缺乏青色光发射,往往会造成显色性能不足。本研究通过传统高温固相法合成了β-Si₅AlON₇:Eu荧光粉,采用X射线衍射仪(XRD)、扫描电镜(SEM)、X射线光电子能谱(XPS)等研究了其结构、形貌、元素和价态。通过光谱仪表征了样品的激发光谱以及发射光谱的波长范围并测试了热猝灭性能,发现激发波长覆盖紫外至蓝色光区域,并且发射光谱显示出典型的Eu²⁺跃迁的宽谱。在300℃下,样品的发射光强度依然可达到室温强度的40%左右,热激活活化能(E_a)达到了3.7 eV,相比较商用YAG:Ce³⁺(YAG)荧光粉,热稳定性有一定的提升。在与蓝色芯片复合后成功制备了高显色(显色指数R_a=87)的白色发光LED,对应的色温也达到了暖白光范围(CCT=4501K)。本研究实现了SiAlON基青色...     

Combustion synthesis of β-SiAlON from a mixture of aluminum ferrosilicon and kaolin with nitrogen-containing additives using acid enrichment

In the work, single-phase β-SiAlON was prepared from a powder mixture based on aluminum ferrosilicon and aluminosilicate (kaolin) with nitrogen-containing additives (product of nitriding of the starting mixture and NH₄F) by combustion synthesis followed by acid enrichment of the synthesized product. Self-propagating combustion synthesis was conducted under natural nitrogen filtration. The synthesis parameters (nitrogen pressure, sample diameter, density of the starting mixture) and the conditions of acid enrichment of the synthesized products (acid concentration, temperature of acid enrichment and dispersion of the starting powder) were determined. After acid enrichment of the synthesized product, which contained β-SiAlON and α-Fe phases, the phase content of β-SiAlON was 99.5 wt%.     

Anomalous upconversion behavior and high-temperature spectral properties of Yb/Ho-SiAlON ceramics

Traditionally, NaYF₄ and glass-based materials are considered the most efficient upconversion materials. However, those materials may show signs of thermal warping or risks of fracture during long-term service life in extreme environments. In contrast, SiAlON ceramics preserve their spectral and physical integrity during continuous use due to their ultra-low thermal expansion coefficient (～3.0 × 10^?6/K) even at extreme temperatures. Here, we investigate the upconversion photoluminescence properties of Ho and Yb co-doped SiAlON (Ho/Yb-SiAlON) ceramics, prepared by hot-press method, at room temperature and at high temperature (298–1023 K). At room temperature, Ho/Yb-SiAlON ceramics show intense red upconversion emission under 980 nm excitation. At the high-temperature range, the spectral shift is absent in Ho/Yb-SiAlON indicating that the SiAlON ceramics have high-temperature spectral stability, which may be attributed to the low thermal expansion coefficient of SiAlON ceramics. Ho and Yb concentration-dependent spectra show an anomalous upconversion emission behavior. It is found that a higher sensitizer and low activator concentration combination is not always an ideal choice for sensitized luminescence in SiAlON ceramics which is in stark contrast to the common understanding of sensitized luminescence. The mechanism involving the dominant cross-relaxation process has been proposed to explain the observed anomalous upconversion behavior.     

Relationship between color changes and ternary eutectic reaction in Yb/Y-co-doped SiAlON ceramics

This study investigated the relationship between the green/brown colors and Yb/Y-co-doped ternary eutectic reactions. A color difference was initially observed at 1600 °C. The green color indicates a relatively highly porous area compared to the brown color, and it was confirmed that the green color was spherical in all samples. This difference in color was analyzed through photoluminescence (PL), and it was confirmed that the reduction of Yb²⁺ increased at temperatures higher than 1550 °C owing to the reducing atmosphere generated by the carbon ambient. The reaction sequence of the phase formation of SiAlON exhibited a difference resulting from the reduction in Yb ions, and the sequence of phase formation improved with an increase in the content of Y substituted for Yb.