孔结构对氮化硅陶瓷介电性能的影响

采用添加成孔剂和冰冻．干燥法制备了具有不同气孔率的氮化硅多孔陶瓷，研究了该陶瓷在9．3GHz的微波介电性能。用SEM对微观形貌进行观察。结果表明，不同的成型工艺制备出具有不用孔结构的氮化硅多孔陶瓷，添加成孔剂制备的多孔陶瓷为较大的孔、洞分布在较致密的基体上；冰冻．干燥法制备的多孔陶瓷具有复合孔结构。对试样介电特性的研究表明，除了气孔率对介电常数和介电损耗有较大影响外，孔结构也是影响其介电特性的重要因素。     

Aluminum doping and dielectric properties of silicon carbide by CVD

Cubic β-SiC coating was grown onto the graphite substrate by the normal pressure chemical vapor deposition using CH3SiCl3 （MTS） as a source precursor at 1 150 ℃. But the hexagonal Al4SiC4 phase was generated in the doped process with trimethylaluminium （TMA） as the dopant. Microstructure of the deposit coating as-prepared was characterized by scanning electron microscope （SEM）, which consists of spherical particles with a very dense facet structure. The real component of permittivity ε＇ and dielectric loss tang of the coatings undoped and doped by TMA were carried out by a vector network analyzer in the microwave frequency ranges from 8.2 GHz to 12.4 GHz. The results show that both of them have low values, and doped coating has lower ε＇ and tan δ than undoped one due to the existence of Al4SiC4 impurity phase, which indicates that the desired Al/SiC solid solution at 1 150 ℃ in a normal argon atmosphere is not produced.     

Microstructure and mechanical properties of silicon nitride with tape cast tri-layer structures

Four kinds of silicon nitride samples with tri-laminate structures were prepared by stacking tapes with aligned β-Si₃N₄ whisker seeds. Three-point flexural strengths of the samples were measured at both room temperature and 1673 K. As the total thickness of the layers with the whisker seeds aligned parallel to tension was increased, the flexural strength was increased at both room temperature and at 1673 K. The flexural strength at 1673 K was more sensitive to orientations of the grains in the surface layer than that at room temperature. Observation of the fracture surface revealed that the grains growing from the neighboring whisker seeds were often broken such that they formed a single one grain. Extensive brittle fracture of the grains without much grain pull-out occurred even at 1673 K for the samples.     

基于包混和复合添加工艺的多孔碳化硅陶瓷的制备和性能

采用包混工艺合成核-壳结构的硅-树脂先驱体粉体,引入Al2O3-SiO2-Y2O3复合添加剂,通过成型、炭化和烧结工艺制备多孔碳化硅陶瓷。分析多孔碳化硅陶瓷样品的物相、形貌、孔隙率、热导率、热膨胀系数和抗热震性能。结果表明：复合添加能够在较低的温度下制得多孔碳化硅陶瓷;陶瓷样品的晶粒较小,明显增强了多孔碳化硅陶瓷的导热性能;复合添加提高了碳化硅陶瓷的抗热震性能,添加Al2O3-SiO2-Y2O3并且在1650℃下烧结制备的多孔碳化硅陶瓷经过30次热震后的抗弯强度损失率为6.5%;陶瓷样品的孔壁更加光滑,孔分布更均匀;复合添加对多孔碳化硅陶瓷热膨胀系数的影响较小。     

热解温度对聚碳硅烷转化SiC陶瓷结构及介电性能的影响(英文)

采用真空高温裂解聚碳硅烷法制备β-SiC陶瓷粉末,并对热解产物进行TGA/DSC、XRD和拉曼光谱表征。通过矩形波导法测量β-SiC陶瓷粉末与石蜡复合材料在8.2~18GHz下的复介电常数来研究其介电性能。结果表明:复介电常数的实部与虚部均随着热解温度的升高而增大。高温下产生的石墨碳引起的电子松弛极化及电导损耗是复介电常数的实部与虚部增大的主要原因。     

Dielectric properties of doped silicon carbide powder by thermal diffusion

The doped SiC powders were prepared by the thermal diffusion process in nitrogen atmosphere at 2 000℃. Graphite film with holes was used as the protective mask, The dielectric properties of the prepared SiC powders at high frequencies were investigated. The complex permittivity of the undoped and doped SiC powders was measured within the microwave frequency range from 8.2 to 12.4 GHz. The XRD patterns show that before and after heat treatment no new phase appears in the samples of undoped and nitrogen-doped, however, in the aluminum-doped sample the AIN phase appears. At the same time the Raman spectra indicate that after doping the aluminum and nitrogen atoms affect the bond of silicon and carbon. The dielectric real part （ε） and imaginary part （ε＂） of the nitrogen-doped sample are higher than those of the other samples. The reason is that in the nitrogen-doped the N atom substitutes the C position of SiC crystal and induces more carriers and in the nitrogen and aluminum-doped the concentration of carriers and the effect of dielectric relaxation will decrease because of the aluminum and nitrogen contrary dopants.     

Fatigue resistant silicon nitride ceramics due to anelastic deformation and energy dissipation

To investigate the link between internal friction and fatigue resistance of sintered silicon nitride at elevated temperatures, impulse excitation, torsion pendulum and uniaxial tension–compression tests were performed. At low stress-amplitudes, an internal friction peak is observed and associated with the glass transition of amorphous intergranular phases (IGPs). This peak constitutes a reliable means of energy dissipation for otherwise brittle ceramics. The high amplitude uniaxial tests have revealed a new and much larger internal friction effect than previously could be expected from low amplitude test results. Rheological analysis indicates that the underlying deformation is truly anelastic. Within the investigated stress-amplitude range (30–150 MPa), the damping is shown to increase linearly with stress-amplitude. As a consequence, energy dissipation in a cyclically loaded component will increase locally at stress concentrations such as crack tips. This results in an increased crack propagation resistance, and explains earlier observations of a positive fatigue effect in sintered silicon nitride at high temperature.     

Sr掺杂对BaTiO3陶瓷结构与介电性能的影响

以BaCO3、SrCO3和TiO2为原料,通过固相烧结方法制备了Ba1-xSrxTiO3(0≤x≤1)。利用X射线衍射仪(XRD)、扫描电镜(SEM)、以及阻抗分析仪分别分析Ba1-xSrxTiO3相结构、显微组织和测量介温谱。结果表明,Sr的掺杂没有改变BaTiO3的晶体结构,Ba1-xSrxTiO3(0≤x≤1)固溶体为完全互溶固溶体,为单一的立方相,但随着锶含量的增加,居里点逐渐降低。     

氮化硅陶瓷超塑性研究

以非晶氮化硅纳米陶瓷粉体为起始材料,以纳米氧化钇和氧化铝为添加剂液相烧结获得超塑性陶瓷块体材料,实现氮化硅陶瓷的超塑性拉伸和超塑性成形。氮化硅陶瓷的平均晶粒直径为280nm,在1550℃的较低温度,4.7×10-4/s的相对较高应变速率下,延伸率可达到110%,在成形速率0.2mm/min的条件下,可拉深成形出完好的球形和锥形零件。在室温断口上存在大量的细小的白色氮化硅晶粒;而高温断口上却几乎不存在这样的晶粒,这种不同可以用氮化硅陶瓷材料的超塑性变形机理来解释,也可以证明超塑性变形过程中晶界玻璃相的存在。     

A closed form solution for laser drilling of silicon nitride and alumina ceramics

A closed form solution has been obtained for laser drilling of silicon nitride (Si₃N₄) and alumina ceramics (Al₂O₃). The drilling of workpiece is performed by using a TEM₀₀ 10 ns pulse Nd:YAG laser. It is assumed that the phase transition from solid to vapor occurs without melting. Considering the absorption of plasma plume formed on the surface of the ceramics, the one-dimensional thermal model is developed in order to describe the drilling process. The governing equation of heat-diffusion is solved analytically using a Laplace transformation method. Erosion depth per laser pulse obtained from the closed form solution agrees with the available experimental data.     

Preparation and mechanical properties of Si2N2O ceramics

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氮化硅陶瓷磨削表面残余应力的测试与计算

利用X射线衍射应力分析的sin2 ψ法测量、计算出氮化硅陶瓷试样的残余应力。分析表明 ,经平面磨磨削后的气压烧结氮化硅陶瓷试样表面存在的残余应力为拉应力 ,而再经过表面抛光处理 ,则可以适当地降低表面残余应力。     

碳纳米管/聚酰亚胺纳米复合材料的制备及动态力学性能和介电性能

依次用混强酸和SOCl2对多壁碳纳米管(MWNTs)进行改性,解决其在有机溶剂的溶解性和在基体聚酰亚胺中分散性问题,并采用光电子能谱(XPS)和透射电镜(TEM)对改性前后的MWNTs进行表征.以4,4'-二氨基二苯醚(ODA)和3,3',4,4'-二苯甲酮四羧酸二酐(BTDA)为原料,以原位聚合法将改性碳纳米管掺杂聚酰亚胺(PI),制备MWNTs/PI纳米复合材料.通过热重分析(TGA)、动态力学分析(DMA)和电容测试对材料的热性能、动态力学和介电性能进行表征.结果表明:加入MWNTs后,材料仍有很好的热稳定性,材料的动态力学性能随MWNTs增加而增强,在50℃和10%(质量分数)MWNTs时储能模量为2.307 GPa,比纯聚酰亚胺(PI)提高23.1%;材料的介电常数随着MWNTs含量的增加明显提高,在IMHz和10%时介电常数为66.7,是纯PI的18.6倍.制备的碳纳米管/聚酰亚胺材料是一种具有优良的热学、动态力学力学和介电性能性能的纳米复合材料.     

成孔剂和硅粉粒度对反应烧结氮化硅性能的影响

以硅粉为原料，通过添加不同含量的成孔剂，反应烧结制备出具有不同气孔率的低密度多孔氮化硅陶瓷，研究了成孔剂含量和硅粉粒度对反应烧结氮化硅性能的影响。结果表明，随着成孔剂含量的增加，试样气孔率变大，强度随之减小，烧结后试样中的α-Si3N4相增多，介电常数实部和介电损耗降低，最低介电常数实部可达到2．4左右；不同粒度硅粉中添加30％（质量分数，下同）成孔剂的坯体烧结，在气孔率保持不变的条件下，初始硅粉粒度越小，烧结后试样强度越大，介电常数实部和介电损耗明显减小。     

Assessment of techniques for characterizing the surface quality of ground silicon nitride

This study evaluates techniques used to detect and quantify the extent of surface and subsurface damage in ground silicon nitride. Specimens of two differently ground surfaces of a hot isostatically pressed (HIP) silicon nitride, commercially designated as GS-44, were subjected to six types of analyses, namely mechanical stylus profiling, atomic force microscopy, point-counting analysis of fragmentation pits, la-ser-light scattering, optical gating, and grazing incidence x-ray diffraction (GIXD). The results of these investigations are compared and discussed. The techniques providing the clearest correlations with grinding conditions were mechanical stylus roughness, fragmentation analysis, and GIXD (residual stress conditions). Those that exhibited some correlation but appear to require more work to develop a reliable evaluation method were laser scattering and optical gating. Atomic force microscopy was useful, but not as a routine investigative tool for quality control in ceramic machining. The techniques that appear to have the most near-term potential for routine use are fragmentation analysis and optical gating. Laser-based optical scattering exhibits potential for routine application, but, more development is needed for its commercialization.     

Study on magnetic and dielectric properties of YMnO3 ceramics

The magnetic and dielectric properties were investigated in the hexagonal YMnO₃ ceramics synthesized by sol-gel method. An antiferromagnetic order about 70 K and a weak ferromagnetic order at 5 K have been detected in YMnO₃ ceramics. In addition, we observed also the exchange-bias (EB) effect at low temperatures and it may originate from exchange coupling at the interface between ferromagnetic and antiferromagnetic orders for the co-existence of these two orders in some temperature region in hexagonal YMnO₃. Furthermore, the dielectric measurements showed two thermally activated relaxation behaviors following the Arrhenius law in 290-430 K and above 500 K in YMnO₃ ceramics and they can be explained as the dipolar effects associated with the charge carrier hopping between Mn²⁺ and Mn³⁺ and oxygen vacancy, respectively.     

多孔类石墨相氮化碳的制备及光催化性能研究

通过简单的氨水水热法制备得到了多孔g-C3N4光催化材料。利用 X 射线衍射（XRD）、红外光谱（FT-IR）、扫描电子显微镜（SEM）、透射电子显微镜（TEM）研究了氨水对多孔g-C3N4结构的影响。并以亚甲基蓝为目标分解物考察了样品的可见光催化活性。研究结果表明：制备得到多孔g-C3N4具有由2D 纳米片和相互连通的孔道组成的多孔纳米结构。多孔g-C3N4的可见光催化活性得到了提升,原因在于相较于普通g-C3N4,多孔g-C3N4能够提供更多的光催化反应活性位点,并且具有更高的光生载流子分离及迁移效率。     

连续氮化硅纤维的氧化行为与高温影响研究

连续氮化硅陶瓷纤维是透波／承载一体化陶瓷基复合材料的关键原材料,也是制约复合材料耐高温性能与力学性能的关键因素。本文系统研究了国防科技大学研制的连续氮化硅纤维的抗氧化性能,分析了高温处理后纤维的组成结构与力学性能变化规律。结果表明：1000°C氧化1h后纤维强度高于原始纤维强度,主要是形成的玻璃相能减少和弥补纤维的表面缺陷。随着空气中处理温度提高,氧含量增加,纤维表面形成的SiO₂层逐渐变厚,纤维强度明显降低。纤维在1200°C氧化1h后强度保留率为63%,表明在此温度以下纤维有较好的服役性能。另一方面,氮化硅纤维在1450°C N₂中处理1h的强度保留率为57%,表现出良好的耐高温性能。纤维表面氧化对其在N₂下的耐高温性能具有不利影响,1000°C氧化的纤维在1450°C处理后丧失强度,1500℃处理后形成氮化硅结晶,失重明显增长,纤维内部也开始产生缺陷。     

Processing and mechanical properties of porous silica-bonded silicon carbide ceramics

A simple processing route for manufacturing highly porous, silica-bonded SiC ceramics with spherical pores has been developed. The strategy adopted for making porous silica-bonded SiC ceramics entails the following steps: (i) fabricating a formed body through a combination of SiC and polymer microbeads (employed as sacrificial templates) and (ii) sintering the formed body in air. SiC particles are bonded to each other by oxidation-derived SiO₂ glass. By controlling the microbead content and the sintering temperature, it was possible to adjust the porosity such that it ranged from 19 to 77%. The flexural and compressive strengths of the porous silica-bonded SiC ceramics with ≈40% porosity were ≈65 MPa and ≈200 MPa, respectively. The superior strengths were attributed to the homogeneous distribution of small (≤30 μm), spherical pores with dense struts in the porous silica-bonded SiC ceramics.