氮化硅晶须对反应烧结氮化硅多孔陶瓷介电性能的影响

以硅粉和氮化硅晶须为原料,通过添加30%(质量分数)成孔剂球形颗粒,以聚乙烯醇作粘结剂,采用干压成型工艺,反应烧结制备了多孔氮化硅陶瓷,分析对比了氮化硅晶须对反应烧结氮化硅多孔陶瓷介电性能的影响.实验结果表明,随着氮化硅晶须加入量的升高,氮化硅多孔陶瓷的介电常数和介电损耗都升高,介电性能恶化.     

包覆成孔剂法制备高性能多孔氮化硅陶瓷工艺

为了制备高强度且分布均匀的氮化硅陶瓷,采用包覆成孔剂法改进普通添加成孔剂的方法,常压烧结氮化硅多孔陶瓷,采用阿基米德法、三点弯曲法分别测试材料的孔隙率及抗弯强度,用扫描电镜和光学放大镜对氮化硅多孔陶瓷显微结构和表观结构进行研究.结果表明,添加包覆过的成孔剂强度比添加未包覆的成孔剂强度高,孔隙率为50%时,强度增加近一倍.强度的提高归因于特殊的微观结构,即气孔的均匀分布和孔与孔之间相间隔分布.     

Indentation fatigue in silicon nitride, alumina and silicon carbide ceramics

Repeated indentation fatigue (RIF) experiments conducted on the same spot of different structural ceramics viz. a hot pressed silicon nitride (HPSN), sintered alumina of two different grain sizes viz. 1 μm and 25 μm, and a sintered silicon carbide (SSiC) are reported. The RIF experiments were conducted using a Vicker’s microhardness tester at various loads in the range 1–20 N. Subsequently, the gradual evolution of the damage was characterized using an optical microscope in conjunction with the image analysing technique. The materials were classified in the order of the decreasing resistance against repeated indentation fatigue at the highest applied load of 20 N. It was further shown that there was a strong influence of grain size on the development of resistance against repeated indentation fatigue on the same spot. Finally, the poor performance of the sintered silicon carbide was found out to be linked to its previous thermal history.     

Crystallite-size-dependent characteristics of porous silicon

Porous silicon prepared with anodic currents of 5 to 30 mA/cm² are characterized for structural and electronic properties of surface using photoluminescence, grazing angle X-ray diffraction, photoconductivity, thermally stimulated exo electron emission and work function measurements. The observed results indicate that with increasing porosity the crystallite size decreases and the amount of silicon hydride and oxide-type species increases, exhibiting a tendency similar to that of hydrogenated amorphous silicon and hydrogenated microcrystalline silicon. Free-standing powder of porous silicon, characterized by bright photoluminescence at 730 nm, showed crystallites of nanometre dimensions under the transmission electron microscope.     

ECR-PECVD制备氮化硅薄膜的键态结构

用红外光谱和拉曼光谱分析了用低温电子回旋共振等离子体CVD技术制备的Si3N4薄膜的键态结构。结果表明Si3N4薄膜主要由Si-N键结构组成,还含有Si-H和Si-O-Si键结构。随着沉积温度的提高,Si3N4薄膜中的Si-H键减少,氢含量降低。可利用提高沉积温度来减少Si3N4薄膜中的氢含量。在沉积温度为420℃时Si3N4薄膜的Raman光谱在短波方向出现一新的展宽的拉曼散射峰。     

Properties of reaction bonded silicon nitride obtained from slip cast preforms

Fabrication of silicon preforms of high green density (>1·2 g/cm³) by slip casting of silicon (in aqueous medium) has been studied. The nitridation product consists of 59–85% α-Si₃N₄, 7–22%β-Si₃N₄ and 7–23% Si₂N₂O phase. The amounts of un-nitrided silicon were negligible. The microstructure is either granular or consists of needle-like grains (α-Si₃N₄) and whiskers deposited in the large pores. MOR values of the specimens are almost constant up to 1000°C or 1400°C or show slight increase up to 1000°C or 1200°C. In some cases a little dip around 1200°C, then a sharp increase in MOR up to 1400°C was observed.K _ic values are almost constant up to 1000°C, and thereafter increase sharply. Pore size distribution, existence of Si₂N₂O phase and oxidation of RBSN at high temperatures have been considered for the explanation of the observed behaviour.     

大气中烧结多孔氮化硅的相变和氧化机理研究

以α—Si3N4为原料，分别以Y2O3-Al2O3和MgO-Al2O3-SiO2两个体系作为烧结助剂，在大气中对氮化硅坯体在1400～1550℃进行烧结。研究了烧结温度、烧结助剂体系对氮化硅的氧化程度、氧化产物的影响。结果表明，以MgO-Al2O3-SiO2作烧结助剂有利于α-Si3N4转变为β-Si3N4，且该烧结助剂体系的的抗氧化能力也明显优于Y2O3-Al2O3体系。氮化硅在不同温度烧结时形成的氧化产物不同。     

Mechanism and control of formation of porous silicon onp-type Si

A simple extension of Beale’s and Lehmann’s models for the formation of porous silicon layer onp-type silicon is proposed with a view to explain the experimental conditions necessary for obtaining either uniform vertical pores or non-uniform pore branching, as desired. A uniformity parameter is defined and correlated with the measured porosity. The dependence of the porosity and the uniformity factor with the various formation parameters of porous layer are studied experimentally and explained qualitatively.     

Patterning of porous silicon nanostructures and eliminating microcracks on silicon nitride mask using metal assisted chemical etching

A method for selective formation of reproducible, high fidelity and controllable nano and micrometer size porous Si areas over n-type Si wafers is provided. A 400 nm thick Silicon Nitride layer was used as the mask layer while Platinum and Palladium nanoparticles were deposited over the unprotected areas to obtain porous areas through metal assisted chemical etching process. Nanoparticles were deposited by electroless plating solutions containing H₂PtCl₆ and PdCl₂. Good controls over pore size and depth were obtained with well defined and sharp edges of the patterned areas. The results were compared to porous structures obtained via electrochemical etching process, indicating the superiority of metal assisted etching in terms of its simplicity as well as the ability of Silicon Nitride layer acting as the mask layer.     

Raman scattering and photoluminescence study of porous silicon formed on n-type silicon

We report Raman scattering and photoluminescence studies on porous silicon film formed on n-type silicon. The Raman spectra over the sample surface exhibit considerable variation whereas the photoluminescence spectra are practically identical. Our results indicate that, well inside the film surface, it consists of spherical nanocrystals of typical diameter ≈ 100Å, while on the edge these nanocrystals are ? 300Å. We further observe that there is no correlation between the photoluminescence peak position and the nanocrystal diameter. This suggests that the origin of the photoluminescence is due to radiative recombination between defect states in the bulk as well as on the surface of the nanocrystal.     

Sintering of nano crystalline α silicon carbide doping with aluminium nitride

Sinterable silicon carbide powders were prepared by attrition milling and chemical processing of an acheson type α-SiC. Pressureless sintering of these powders was achieved by addition of aluminium nitride together with carbon. Nearly 99% sintered density was obtained. The mechanism of sintering was studied by scanning electron microscopy and transmission electron microscopy. This study shows that the mechanism is a solid state sintering process.     

Effect of solid content on pore structure and mechanical properties of porous silicon nitride ceramics produced by freeze casting

Porous Si₃N₄ ceramics were prepared by freeze casting using liquid N₂ as refrigerant. The pore structure, porosity, α → β-Si₃N₄ transformation and mechanical properties of the obtained materials were strongly affected by the solid contents of the slurries. Increasing the solid content would reduce the porosity, decrease the pore size and change the pore structure from the aligned channels with dendrites to the round pores with decreased pore size. The formation of this round pores impeded the α → β-Si₃N₄ phase transformation, but was beneficial to the mechanical properties of the obtained porous Si₃N₄ due to its unique pore structure.     

Determination of Vickers microhardness on porous silicon surfaces

The Vickers microhardness values of two different sets of porous silicon layers were determined at applied load of 98 mN. The sets consisted of Boron-doped substrates anodized at diverse current densities for two different amounts of hydrofluoric acid (HF) in the etching solution. We found that the microhardness of the samples with lower content of HF at the anodization process showed higher values, whereas the Vickers parameter diminishes consistently for higher current densities. A possible explanation of this behavior is proposed.     

Preparation of zirconium pyrophosphate bonded silicon nitride porous ceramics

Abstract

A new method for preparing high bending strength porous silicon nitride ceramics with controlled porosity was developed using a pressureless sintering technique, using zirconium pyrophosphate as a binder. The fabrication process was described in detail and the sintering mechanism of porous ceramics was analysed by an X-ray diffraction method. The microstructure and mechanical properties of the porous Si₃N₄ ceramics were investigated, as a function of the content of ZrP₂O₇. The resultant porous silicon nitride ceramics sintered at low temperature (1000 and 1100°C) showed fine micropore structure and a high bending strength. Porous silicon nitride ceramics with porosity of 34–47%, a bending strength of 40–114 MPa and a Young's modulus of 20–50 GPa were obtained.     

Optical sensing of flammable substances using porous silicon microcavities

A porous silicon multilayer, constituted by a Fabry–Pèrot cavity between two distributed Bragg reflectors, is exposed to vapor of several organic species. Different resonant peak shifts in the reflectivity spectra, ascribed to capillary condensation of the vapor in the silicon pores, have been observed. Starting from experimental data, the layer liquid volume fractions condensed in the sensing stack have been numerically estimated. Values ranging between 0.27 (for ethanol) and 0.33 (for iso-propanol) have been found. Time-resolved measurements show that the solvent identification occurs in less then 10 s.     

制备温度对多孔硅光学特性的影响(英文)

本文不同的温度下制备多孔硅.通过荧光光谱、光吸收谱、X射线光电子谱研究了多孔硅的光和结构特性.研究结果表明存在着一个制备临界温度343 K,当制备温度从临界温度之下提高到临界温度之上时,多孔硅的荧光和光吸收从红移转向蓝移,同时硅2p电子结合能也从减小转向增大.     

The potential of porous silicon gas sensors

Recent developments in porous silicon gas sensors have been reviewed. Monitored species detection levels, and the mechanisms of sensing for different sensor designs are also discussed. Porous silicon surface modification methods have been employed for detecting different gas molecules; H₂O, ethanol, methanol, isopropanol, CO_x, NO_x, NH₃, O₂, H₂, HCl, SO₂, H₂S and PH₃.     

Fracture behavior of silicon nitride ceramics subjected to hypervelocity impact

A new advanced ceramic thruster made of monolithic silicon nitride ceramics was developed for the planetary exploration spacecraft AKATSUKI (PLANET-C) at Institute of Space and Astronautical Science (ISAS), Japan Aerospace Exploration Agency (JAXA). To ensure its operation onboard the spacecraft, the reliability of the ceramic thruster against micrometeoroid hypervelocity impact has been investigated. Silicon nitride plates were impacted by spheres of stainless-steel and other materials with 0.2-0.8-mm diameters in the velocity range up to 8.0 km/s using a two-stage light-gas gun. Using crater depth data under various impact conditions, the penetration equation of silicon nitride was determined. The impacted samples showed fracture patterns of three types: cratering, cratering with spallation, and perforation. These fracture patterns were well categorized by the multiple forms of the penetration equation.