Synthesis and characterization of submicron silicon carbide powders with silicon and phenolic resin

A novel three-step process is used to fabricate submicron silicon carbide powders in this paper. The commercially available silicon powders and phenolic resin are used as raw materials. In the first step, precursor powders are produced by coating each silicon powder with phenolic resin shell. Then, precursor powders are converted into carbonized powders by decomposing the phenolic resin shell. The submicron silicon carbide powders are formed in the reaction of silicon with carbon during the third step of thermal treatment. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD) and thermogravimetric (TG) analyses are employed to characterize the microstructure, phase composition and free carbon content. It is found that the sintered powders consist of β-SiC with less than 0.2 wt.% of free carbon. The particle size of the obtained silicon carbide powders varies from 0.1 to 0.4 μm and the mean particle size is 0.2 μm. The silicon carbide formation mechanism of this method is based on the liquid-solid reaction between liquid silicon and carbon derived from phenolic resin. The heat generated during the reaction leads to great thermal stress in silicon carbide shell, which plays an important role in its fragmenting into submicron powders.     

Densification of surface-modified silicon carbide powder by spark-plasma-sintering

SiC was densified by spark plasma sintering (SPS) and the effects of surface modification of the powder particles on its sintering behavior were investigated. The pressure and temperature conditions were set to 50 MPa and 2200 °C, respectively. Specific SPS experiments at a lower temperature (i.e. 1600 °C) was performed to analyze the efficiency of the sintering and the early stage of the densification in softer conditions. The surface functionalization was carried out by grafting a thin molecular layer of a preceramic precursor on the grain surface of SiC particles, which acts as a sintering additive without producing contamination by heteroatoms since, in addition to hydrogen, it contained only Si and C in the same ratio 1:1 as silicon carbide. One of the advantages of this surface functionalization is that it reduces the temperature at which the sintering process begins and therefore it facilitates and increases the densification of the final SiC parts.     

利用稻壳合成SiC的研究

稻壳经细粉碎、酸处理、FeCl2·6H2O浸泡、过滤、干燥、高温分解与合成、HF溶液处理,即可得到SiC含量50％～70％的合成碳化硅。     

氮化硅结合碳化硅耐火材料的氧化

氮化硅结合碳化硅耐火材料高温氧化后，其抗折强度有所提高，但经扫描电镜观察，材料断面结构已发生了明显的变化。该材料长时间在氧化气氛中使用，可靠性将下降。     

氮化硅结合碳化硅树料的抗渣侵蚀性

借助光学显微镜、扫描电子显微镜和Ｘ射线衍射分析等手段，研究了矿渣侵蚀后的氮化硅结合碳化硅材料的显微结构和物相组成．探讨了氮化硅结合碳化硅材料的损坏机理。     

Influence of mechanical activation on combustion synthesis of fine silicon carbide (SiC) powder

The influence of mechanical activation of powder mixtures of Si and C, via high energy attrition milling (up to 12 h), on combustion synthesis of SiC was experimentally investigated. β-SiC fine powder was successfully fabricated in 1.0 MPa N₂ atmosphere without other additional treatments, such as preheating, electric action, or chemical activation. Relatively weak peaks of α-SiC, α-Si₃N₄ and Si₂ON₂ were also found in the final products. The experimental results and their theoretical treatment showed that mechanical activation via high energy ball-milling provides to the initial Si/C powder mixture extra energy, which is needed to increase the reactivity of powder mixture and to make possible the ignition and the sustaining of combustion reaction to form SiC.     

氮化硅结合碳化硅耐火材料在钢水中的腐蚀行为

运用扫描电镜（ＳＥＭ）技术，研究了氮化硅结合碳化硅耐火材料在钢水中的腐蚀行为。结果表明，金属与氮化硅结合碳化硅材料之间的界面清晰，基体内部无任何金属渗入，但氧化的材料表面有氧化物粘附。     

氮化物结合碳化硅耐火材料的研究现状

分别概述了以氮化硅、赛隆和氧氮化硅作为结合相 的SiC材料的结构特点、理化性能、生产工艺和应用情况,详细 介绍了国内这3种材料的研究现状,并对今后氮化物结合SiC 材料的研究内容提出了自己的观点。     

氧氮化硅结合碳化硅制品的生产与使用

以工业用黑色碳化硅砂、硅粉为主要原料，研制出了导热性能优良、抗热震性好、耐高温、耐侵蚀及耐磨损，且生产工艺较简单、成本较低的氧氮化硅结合的碳化硅制品．该产品已广泛应用于冶金炉、化工设备及发电用锅炉的内衬，并取得了较满意的效果。     

A perspective on non-stoichiometry in silicon carbide

The non-stoichiometric ceramics are amazing materials with potential to offer applications that are unachievable by using otherwise ideal stoichiometric counterparts. These materials have contributed in wide areas including superconductivity, optical, magnetic, electronic, structural, mechanical and transport applications. The deviation form stoichiometry in a large number of compounds, though usually avoided, has numerous benefits; by increasing ionic conductivity, offering band structure modifications, causing paramagnetic to ferromagnetic transitions, reducing magnetoresistance, increasing mechanical strength, enhancing electrochemical efficiency etc. Keeping in mind the promising contributions of silicon carbide among family of ceramic materials, this review highlights the implications of non-stoichiometry and its properties. The non-stoichiometry produced unintentionally or purposefully is strongly influenced by synthesis conditions and varies for silicon carbide grown in amorphous, crystalline, polycrystalline polytypes in the form of bulk, surfaces and low dimensional structures. The prospects of tuning the properties of silicon carbide on the basis of fabrication of silicon rich and carbon rich by monitoring silicon to carbon ratio are discussed in detail.     

反应烧结SiC材料的高温氧化行为研究

研究了反应烧结SiC材料在 110 0℃空气中的高温氧化行为。结果表明 :反应烧结SiC在110 0℃的氧化动力学曲线符合抛物线规律 ;材料的氧化受O2 和CO在玻璃态硅酸盐中的扩散所控制 ;材料中的杂质元素降低了SiO2 氧化膜的粘度 ,促进了O2 和CO在氧化膜中的扩散     

Improving specific stiffness of silicon carbide ceramics by adding boron carbide

A strategy for improving the specific stiffness of silicon carbide (SiC) ceramics by adding B₄C was developed. The addition of B₄C is effective because (1) the mass density of B₄C is lower than that of SiC, (2) its Young’s modulus is higher than that of SiC, and (3) B₄C is an effective additive for sintering SiC ceramics. Specifically, the specific stiffness of SiC ceramics increased from ~142 × 10⁶ m²?s^?2 to ~153 × 10⁶ m²?s^?2 when the B₄C content was increased from 0.7 wt% to 25 wt%. The strength of the SiC ceramics was maximal with the incorporation of 10 wt% B₄C (755 MPa), and the thermal conductivity decreased linearly from ~183 to ~81 W?m^?1?K^?1 when the B₄C content was increased from 0.7 to 30 wt%. The flexural strength and thermal conductivity of the developed SiC ceramic containing 25 wt% B₄C were ~690 MPa and ~95 W?m^?1?K^?1, respectively.     

Electrochemical corrosion of silicon carbide ceramics in sodium hydroxide

Sintered silicon carbide ceramics have found widespread use due to their high corrosion stability. This corrosion stability can be affected by electrochemical processes. Electrochemical corrosion experiments conducted on an SSiC material in NaOH at different voltages and subsequent detailed investigation of the formed surfaces were carried out. Systematic local measurement of the corrosion rate was carried out using the AFM technique. The results revealed the recession of the SiC grain surfaces under anodic electrochemical loading, with the extents differing strongly from grain to grain. The recession rates were not found to correlate with the SiC grain orientations or polytypes. Rather, the data and the observed microstructure indicated that the behaviour was caused by variations in the resistivities of the grain boundaries.     

Growth of silicon carbide nanotubes in arc plasma treated silicon carbide grains and their microstructural characterizations

Silicon carbide nanotubes were found to grow in straight as well as curved configurations by treating silicon carbide grains in an arc plasma reactor/furnace followed by 3 h of cooling (in air). By increasing the plasma treatment time from 16 min to 20 min, multi-wall tubes were found to change to single wall tubes with reduction in diameter from few nm to sub-nm. Typical in situ grown nanotubes were characterized by XRD, TEM, SAED, HRTEM, EDS and micro Raman spectroscopy, and it is established from these evaluations that the nanotubes are made up of silicon carbide and not carbon. A possible mechanism, involving reaction between the plasma dissociated carbon (solid) forming carbon nanotube and the left-out silicon (existing in vapour state) during the cooling period (3000–2680 °C), is suggested to be responsible for silicon carbide nanotube formation in the plasma assisted process.     

浅谈碳化硅制品形状设计的改进

应根据碳化硅制品的独特性能和制品的实际工作需要来设计形状和尺寸。文中的建议简而易行；本设计对节约资源、提高经济效益、减轻炉体结构重量、延长炉衬使用寿命，对促进经济发展有着重要意义。     

Evaporation-condensation derived silicon carbide membrane from silicon carbide particles with different sizes

Silicon carbide ceramic is a promising membrane material because of the high corrosive and high temperature resistance, and the excellent hydrophility. Here, a silicon carbide ceramic membrane with both substrate layer and separate layer composed of pure silicon carbide phase was successfully prepared. The effect of particle size on the microstructure and properties was investigated. The substrates were prepared from three silicon carbide particles at 2200 ℃. With the content increase of fine particle, the average pore size increased from 5.6 μm to 14.1 μm; meanwhile, the flexural strength of the substrate increased from 14.1 MPa to 24.6 MPa. The separation layers were made from particles of 3.0 μm and 0.5 μm. When sintered at 1900 ℃, the separation layer formed pore network with homogeneous structure. Such silicon ceramic membrane can be used in harsh conditions, including high temperature wastewater and strongly corrosive wastewater.     

含铝粉的MgO-SiC材料对IF钢硅含量的影响

以电熔镁砂、碳化硅和铝粉为主要原料,采用热固性酚醛树脂为结合剂,以等静压(200 MPa)压制成坩埚,自然养生24 h后于230℃保温24 h热处理。随后在坩埚中加入5 kg的IF钢和120 g保护渣,然后放入感应炉中加热至1 600℃至钢水熔化,分别冶炼30 min、60 min、90 min、120 min和180 min后各取1份钢样,化验钢样中的硅含量,并对试验后试样与钢水的反应层进行XRD、SEM和EDAS分析。结果表明:耐火材料和钢液反应层中MgO-CaO-SiO2液相的形成有利于降低材料中SiC对钢水的增Si作用,而铝粉的加入会促进MgO-SiC材料中的SiC向钢中溶解。     

Electrochemical corrosion of silicon carbide ceramics in H2SO4

Sintered silicon carbide materials have found widespread use due to their high corrosion stability. This corrosion stability can be affected by electrochemical processes. Electrochemical corrosion experiments conducted on a SSiC material in H₂SO₄ at different voltages and subsequent detailed investigation of the formed surfaces was carried out. The first time a systematic local measurement of the thickness of the oxide layers was carried out. The measurements revealed the formation of SiO₂ surface layers with thickness up to 125 μm. The measured values also showed a strong deviation from grain to grain. The thickness of the layers does not correlate with the crystallographic orientation of the grains or the SiC-polytypes. The data indicate that the behaviour is caused by the variation of the resistivity of the grain boundaries. The measured thicknesses as a function of the electrical charge transferred indicate that the electrochemical oxidation results in the SiO₂ and carbon dioxide.     

Corrosion resistance of silicon-infiltrated silicon carbide (SiSiC)

Silicon carbide ceramics have found widespread use due to their high corrosion stability. Both solid state-sintered silicon carbide, which has an extremely high corrosion resistance, and silicon-infiltrated silicon carbide are used for various applications. The latter material contains SiC as well as free silicon, which is less stable. Hence, in the present work, the corrosion behavior of silicon-infiltrated silicon carbide ceramics was investigated in NaOH solutions. Long-term corrosion experiments were conducted, and a method for analyzing the corrosion behavior in short-term experiments was developed. The short-term method is based on the accurate measurement of the corrosion depth by laser scanning microscopy on polished surfaces. The results of both methods were in good agreement. The advantage of the short-term method is that it provides information on changes in corrosion mechanisms and corrosion rates in the initial period and as a function of the impurities present. Preferential corrosion of Si at the interface to SiC was observed. TEM investigations revealed that this enhanced corrosion was caused by the segregation of impurities.     

石灰粉在密闭电石炉生产中的应用

为了利用电石生产厂家筛分分离出的大量石灰粉末,浙江巨化电石有限公司成功地将其应用于埃肯型密闭电石炉炉心生产电石。通过3个月的试验,结果表明,使用石灰粉末后,电石优一级产品率上升了2.32%,日产量增加了6.6 t,密闭炉电石电耗下降了102 kWh/t,投炉石灰消耗也下降了38 kg/t,电石生产成本大幅降低,设备故障也明显减少。