氮化硅粉体的表面化学性质和水中的胶体特性

陶瓷粉体的表面性质和胶体行为对成型、烧结等工艺过程有很大影响。本文回顾了近年来对氮化硅粉体的表面化学性质和水中的胶体特性的研究成果。系统介绍了氮化硅粉体表面元素的键合状态、表面官能团、氧在颗粒表面和内部的分布和表面富氧层的厚试行表面化学性质,以及氮化硅颗粒在水中的荷电机理、等电点和Ｚｅｔａ电位与表面氧含量的关系、含烧结助剂氮化硅多相体系的胶体特性和分散剂的作用机理等胶体特性。     

氮化硅陶瓷的制备及性能研究进展

氮化硅陶瓷是一种具有广阔发展前景的高温、高强度结构陶瓷,它具有强度高、抗热震稳定性好、疲劳韧性高、室温抗弯强度高、耐磨、抗氧化、耐腐蚀性能好等高性能,已被广泛应用于各行业。本文介绍了氮化硅陶瓷的基本性质．综述了氮化硅陶瓷的制备工艺和提高其高温性能的方法以及增韧的途径,并展望了氮化硅陶瓷的发展前景。     

Highly porous silica foams prepared via direct foaming with mixed surfactants and their sound absorption characteristics

The highly porous silica ceramics were fabricated by direct foaming with mixed surfactants and the influence of silicon nitride addition and solid content on the microstructures and properties were investigated. The results showed that silicon nitride can impede the formation of cristobalite and facilitates the sintering of silica ceramics. When the addition of silicon nitride powders reached 15 wt%, the highest compressive strength of silica ceramic foams could be obtained. The porosity of silica ceramic foams was tailored in the range of 84.61%–91.35% by adjusting the solid content, and the compressive strength of the obtained ceramic foams ranged from 5.89 MPa to 0.94 MPa. Sound absorption characteristics of silica ceramics foams were investigated. With the porosity of ceramic foams increased from 84.61% to 91.35%, the sound absorption coefficients in the entire sound wave frequency were enhanced due to the reduction of flow resistances, besides, the sound absorption peak varied from 4200 Hz to 2300 Hz, and became more intense and sharper.     

Preparation of Dense Ceramics Based on Silicon Nitride Nanopowders

Synthesis of ceramics from silicon nitride nanopowders using hot-pressing and pressure-assisted and microwave (MW) sintering techniques has been studied. Dense ceramics with improved physicomechanical characteristics can be prepared on condition that most of the oxygen in the form of silicon monoxide (contained at 5 – 8 wt.% in the precursor powders) has been removed from the material. In ceramics treated by the three sintering technologies, an extensive grain growth is observed. The microstructure of these materials was more disperse in comparison with that of ceramic prepared from conventional -Si₃N₄ powders synthesized in a furnace. This provides a route towards preparing nanopowder-based ceramics with a 25 – 30% increase in strength in comparison to ceramics of the same density prepared from conventional powders.     

Silicon nitride/boron nitride ceramic composites fabricated by reactive pressureless sintering

Using Si and BN powders as raw materials, silicon nitride/hexagonal boron nitride (Si₃N₄/BN) ceramic composites were fabricated at a relatively low temperature of 1450 °C by using the reaction bonding technology. The density and the nitridation rate, as well as the dimensional changes of the specimens before and after nitridation were discussed based on weight and dimension measurements. Phase analysis by X-ray diffraction (XRD) indicated that BN could promote the nitridation process of silicon powder. Morphologies of the fracture surfaces observed by scanning electron microscopy (SEM) revealed the fracture mode for Si₃N₄/BN ceramic composites to be intergranular. The flexural strength and Young's modulus decreased with the increasing BN content. The reaction-bonded Si₃N₄/BN ceramic composites showed better machinability compared with RBSN ceramics without BN addition.     

Hierarchical Structure of Porous Silicon Nitride Ceramics with Aligned Pore Channels Prepared by Ice‐Templating and Nitridation of Silicon Powder

A unique hierarchical porous structure of silicon nitride ceramic with 76.5% porosity is fabricated by combining an ice‐templating method and nitridation for a silicon powder. The porous silicon nitride ceramics were composed of a lamellar structure with aligned pore channels and ceramic walls filled with fibrous whiskers. This study is focused on the influences of freezing rate on the microstructures and properties of the silicon nitride ceramics. The properties were characterized by compressive strength and gas permeability, which were shown to vary with controlled microstructure. The compressive strength and the permeability reached up to 32.2 MPa and 0.035^?12 m², respectively.     

Evaluation of oxygen content on silicon nitride powder surface from the measurement of the isoelectric point

The oxygen content associated to the surface of silicon nitride powder particles was characterized using a method which is based on the measurement of the specific surface area and the isoelectric point in aqueous solution. From the dissociation model of hydrolyzed surface groups a linear dependence between the fraction of silanol groups (SiOH) and the pH of the isoelectric point is predicted, which was confirmed by electrophoretic measurements of various commercial silicon nitride powders. The proposed method provides rapid information on the particle surface composition, which is of particular relevance for colloidal processing of silicon nitride powders.     

加入纳米氮化硅对氮化硅陶瓷性能与结构影响

本文以亚微米级氮化硅为起始原料，加入纳米氮化硅来增强基体，添加氧化铝和氧化钇为烧结助剂，等静压成型，采用无压烧结的方式来制备具有优良性能的氮化硅陶瓷。主要研究了纳米氮化硅的分散；纳米氮化硅的加入量对氮化硅陶瓷力学性能的影响；纳米氮化硅的加入量对氮化硅陶瓷使用性能的影响；纳米氮化硅的加入量对氮化硅陶瓷显微结构的影响。研究结果表明：乙醇作为溶剂在分散介质为聚乙二醇的情况下，超声波震荡40分钟时，纳米氮化硅分散效果最好；随纳米氮化硅加入量的增加，显气孔率增加，吸水率增大；加入3wt％的纳米氮化硅时，试样的体积密度最大，抗弯强度、洛氏硬度、断裂韧性最好，具有较理想的显微结构。     

Fabrication and mechanical properties of nacre-like alumina with addition of silicon nitride

How to deal with the brittleness of ceramic materials is always one of the hot topics in the field of materials science. Design of layered ceramics with textured structure is one of the effective methods to improve their fracture toughness. The introduction of additives as interlayer phases can balance fracture toughness and flexural strength. However, the research about addition of interlayer phases and their mechanisms in the layered ceramics is still limited. In this work, nacre-like alumina ceramics were successfully fabricated by freeze casting followed by hot pressing. Silicon nitride was incorporated as the interlayer phase, and the effect on the mechanical properties of the nacre-like alumina was investigated. The addition of silicon nitride was beneficial to improvement of interlayer bonding between the alumina layers due to formation of sialon phase, leading to increase of flexural strength but decease of fracture toughness. When the content of silicon nitride was 3.3 wt%, flexural strength and fracture toughness of the sample was 468 MPa and 6.2 MPa m^1/2, respectively. Compared with the sample without silicon nitride, the flexural strength was enhanced significantly. Additionally, both flexural strength and fracture toughness were improved as compared the sample without any additives. This work can provide available references for design and fabrication of high-strength and high-toughness ceramics by properly tuning the layer structure and interlayer phase composition.     

α-β Sialon Ceramics Made from Different Silicon Nitride Powders

The present work is concerned with the sintering of an α-β sialon ceramic using five different silicon nitride powders from a single source. The parameters varied in the silicon nitride were the amount of "free' silicon, iron content, α:β ratio, and grain size as measured by BET surface. The sintering atmosphere was varied by use of protective powder beds with passive (boron nitride) and active (SiO-generating) properties. Five sintering temperatures between 1600° and 1800°C were used. Microstructural characterization as well as density, hardness, and fracture toughness measurements were carried out. The sintering conditions were found to be critical for obtaining fully dense materials and low weight change. The optimum sintering temperature was 1750°C. The silicon nitride powder with a high content of free silicon resulted in a material which was more susceptible to the sintering atmosphere conditions. An α-β sialon made from a silicon nitride powder with a high β-α phase ratio resulted in a higher β-α ratio in the sintered material.     

氮化硅陶瓷在四大领域的研究及应用进展

氮化硅陶瓷不仅具有较高的力学性能还具有良好的透波性能、导热性能以及生物相容性能,是公认的综合性能最优的陶瓷材料。作为轴承球的致密氮化硅陶瓷广泛应用在机械领域;作为透波材料的多孔氮化硅陶瓷广泛应用在航空航天领域;随着对氮化硅陶瓷材料的深入研究,其在导热性和生物相容性方面的优异特性逐渐被科研工作者认识并得到开发和应用。本文详细阐述了氮化硅粉体的制备方法,并综述了氮化硅陶瓷作为结构陶瓷在机械领域和航空航天领域的研究进展,此外还介绍了其作为功能陶瓷在半导体领域、生物制药领域的研究和应用现状,最后对其未来发展进行了展望。     

Fabrication of Si3N4 preforms from Si3N4 produced via CRN technique

Ceramic preforms with randomly distributed particles as reticulated porous structure which are generally used for metal infiltration as reinforcement, membranes, catalyst supports etc. Preforms are characterized by open porosity making possible their infiltration by liquid metal alloys. In this work, quartz powders using carbon black as a reducing agent were used for alpha Si₃N₄ powders synthesis through a carbothermal reduction and nitridation (CRN) process. The CRN process was carried out under nitrogen flow at 1,450 °C for 4 h. At high temperatures, carbon as reducing agent reacts with the oxygen of SiO₂, and the resulting metallic silicon compounds with nitrogen gas to obtain silicon nitride powder. The reacted powders were used to obtain reticulated ceramic by replica method. The powders containing various bentonite ratios were mixed in water to prepare slurry. The slurry was infiltrated into a polyurethane sponge. A high porous ceramic foam (preform) structure was achieved after burn out of the sponge. All ceramic preforms were sintered to increase stiffness (in the temperature range 900–1,350 °C). The sintered ceramic foams were subjected to compressive tests. The scanning electron microscopy was used to examine the reticulated ceramic foam structure, and X-ray diffraction analysis was performed to determine phases.     

Synthesizing high α-phase Si3N4 powders containing sintering additives

Fine grain α-phase silicon nitride (Si₃N₄) ceramic powders were produced via carbothermic reduction of colloidal SiO₂, which contained pre-mixed additives of sintering aids primarily consisting of oxides such as MgO and Y₂O₃. The powders that were pre-mixed in the starting reactants were chosen based on the final powder composition and on type and amount of the secondary phases desired for sintering. After synthesizing, powder properties were examined using standard characterization techniques (XRD, SEM, BET, etc). This technique of ceramic synthesis has advantages in providing nitride-based ceramic powders, which contain secondary in situ phases that are distributed as sintering additives. Silicon nitride ceramic powders synthesized using this method might therefore be readily sintered because the homogeneously distributed sintering additives were present in the starting materials. In this work, the processing parameters are described in terms of the synthesis conditions.     

烧结助剂对多孔氮化硅陶瓷的力学性能及介电性能的影响

通过添加烧结助剂,采用常压烧结工艺制备出不同气孔率(19%～54%)的氮化硅陶瓷.采用Archimedes法、三点弯曲法和Vickers硬度测试法测量了材料的密度、气孔率、抗弯强度及硬度.用X射线衍射及扫描电镜检测了相组成和显微结构.用谐振腔法测试了氮化硅陶瓷在10.2 GHz的介电特性.结果表明:材料具有优良的介电性能.随着烧结助剂的减少,样品中气孔率增加,力学性能有所下降,介电常数和介电损耗降低.添加Lu2O3所制备的氮化硅陶瓷的力学性能和介电性能优于添加Eu2O3或Y2O3制备的氮化硅陶瓷.当气孔率高于50%时,多孔氮化硅陶瓷(添加入5%的Y2O3或Lu2O3,或Eu2O3,质量分数)的抗弯强度可达170 MPa,介电常数为3.0～3.2,介电损耗为0.000 6～0.002.     

Foaming mechanism of polishing porcelain stoneware tile residues via adding C,Al and Si powder

Polishing porcelain stoneware tile residues (PPR) is used to prepare foamed ceramic to solve the problem of solid waste discharge in ceramic industry. In this study, C, Al and Si powder were added to the simulated PPR to control foaming, and the mechanism of silicon carbide foaming in the PPR was discussed in detail. After these powders were introduced into the simulated PPR, the phenomenon of alumina crystallization on the pore wall of the foamed ceramic and the diffusion of gas in the foamed ceramic were discovered to be exciting. The foaming mechanism of PPR is detailed as follows: the diffusion rate of oxygen in silicate liquid is faster than that of CO during sintering, so the CO generated by incomplete oxidation of silicon carbide in PPR accumulates in the liquid, which makes the volume of ceramics expand and causes foaming.     

Thermal transformation of nanohafniumcarbosilanes

The process of thermochemical transformation of nanohafniumcarbosilane (nano-HfCS) at 1500?°C in various media was investigated. The regularities of the formation of SiC ceramic structures modified with hafnium compounds were analyzed by physicochemical methods.The two-stage thermochemical transformation of nano-HfCS first at 1100?°C in argon and then at 1500?°C in various media: argon, nitrogen, vacuum, air results in formation of a nanocrystalline α-SiC ceramics with a hexagonal crystal lattice, modified with HfC, as the main phase. It is demonstrated that the medium in which pyrolysis of nano-HfCS is carried out at 1500?°C affects only the surface layer of the resulting ceramics: at pyrolysis in argon, carbon oxides and hafnium are produced as additional phases on the surface; in nitrogen, silicon nitride and carbon are formed as additional phases on the surface, and in air SiO₂ and carbon are formed on the surface as additional phases.     

Properties of calcium phosphates ceramic composites derived from natural materials

In this study, ceramics containing mixed phases of hydroxyapatite/beta-tricalcium phosphate (HA/β-TCP) were fabricated by a solid-state reaction technique. The HA powder was synthesized from cockle shells while the β-TCP powder was synthesized from egg shells. Pure HA and β-TCP fine powders were successfully obtained. The HA and β-TCP were mixed and subjected to a thermal treatment up to 1100 °C. To form the mixed phase ceramics, the resulting powders were sintered at 1350 °C. Effects of HA concentration on the properties of the studied ceramic were investigated. X-ray diffraction analysis revealed that all samples presented multiphase of calcium phosphate compounds. Average grain size of the ceramics decreased with the HA additive content. The 75 wt% HA ceramic showed the maximum hardness value (5.5 GPa) which is high when compared with many calcium phosphate ceramics. In vitro bioactivity test indicated that apatite forming increased with the HA additive content. To increase antibacterial activity, selected ceramics were coated with AgNO₃. Antibacterial test suggested that an Ag compound coating on the ceramics could improve the antibacterial ability of the studied ceramics. In addition, the antibacterial ability for the Ag coated ceramics depended on the porosity of the ceramics.     

Oxygen Interaction with Hexagonal OsB2 at High Temperature

The stability of ReB₂‐type hexagonal OsB₂ powder at high temperature with oxygen presence has been studied by thermogravimetric analysis, differential scanning calorimetry, SEM, EDS, and high‐temperature scanning transmission electron microscopy and XRD. Results of the study revealed that OsB₂ ceramics interact readily with oxygen present in reducing atmosphere, especially at high temperature and produces boric acid, which decomposes on the surface of the powder resulting in the formation of boron vacancies in the hexagonal OsB₂ lattice as well as changes in the stoichiometry of the compound. It was also found that under low oxygen partial pressure, sintering of OsB₂ powders occurred at a relatively low temperature (900°C). Hexagonal OsB₂ ceramic is prone to oxidation and it is very sensitive to oxygen partial pressures, especially at high temperatures.     

Synthesis and characterization of holmium doped lithium niobate powders

Holmium doped lithium niobate (LN:Ho) powders with initial concentration of holmium in the range 0–7 mol% were synthesized by the ceramic powder processing method. Niobium penta-oxide Nb₂O₅, lithium carboxide LiCO₃ and holmium oxide Ho₂O₃ with a purity of 99.99% were the starting materials. The phase content and lattice parameters of powders and ceramic pellets were characterized by X-ray diffraction (XRD). To further investigate the quality of the synthesized LN:Ho powders, the scanning electron microscopy (SEM) was used to determine the particle size and the morphology. The main results of this work point out the fact that the ceramic powder processing method is a well adapt method for obtaining high quality LN:Ho ceramics in the holmium concentration range analysed as the LiNbO₃ phase is lonely present in the ceramics at the end of the synthesized process and as their grain sizes are regular, with a maximum for the sample doped with 7 mol% of holmium.     

A Nanocomposite Ceramic Based on the Powder of a Carbon-In-Silicon Carbide Solid Solution

The synthesis of a nanocomposite powder of a solid solution of carbon in silicon carbide with controlled content of nitride phases is considered. A method of activated sintering for molding a pore-free nanocomposite ceramic with superior mechanical properties is proposed. Microstructure of the sintered ceramic is examined.