碳热还原法低温合成SiC粉末的研究

研究了碳热还原法低温合成SiC粉末。对SiC-C系统进行了热力学分析以指导合成工艺。研究了合成温度、保温时间、SiO2/C配比等对合成SiC粉末的影响,并对合成SiC粉末的成型性能和烧结性能进行了研究,在此基础上制定出较为合理的合成工艺制度。由此制得晶粒尺寸约为0.1um,二次粒径小于0.5um的烧结性能较佳的β-SiC粉末。     

β—SiC晶须的合成及生长机理

以高岭土、超细碳粉为原料,采用碳热还原方法合成出性能良好的β—SiC晶须,并研究了碳粉加入量、烧成温度对β—SiC晶须产率的影响。结果表明,烧成温度1500～1600℃,碳粉加入量4～10％(wt)为较好的晶须合成条件。该方法制备β—SiC晶须的生长机理为“VS”机理。     

氮化工艺对微波碳热还原法合成AlN粉末的影响

根据微波加热特点,选择合适的合成氮化工艺,合成出优质的AlN,并探讨了在微波环境下各种因素对合成AlN粉末的影响.结果表明,采用合适的微波合成氮化工艺合成AlN,不但在节能省时方面效果显著,而且在合成质量上也有较大的改善.     

反应原料对微波碳热还原法合成AlN粉末的影响

根据微波加热特点,选择合适的反应原料,合成出优质的AlN粉末.结果表明,采用合适的反应原料微波合成AlN,由于微波的"非热效应"以及微波环境下整个反应系统的均匀加热,降低了反应温度,缩短了反应时间,极大的减少了合成成本.     

β-SiC晶须的生长及微观结构研究

以高岭土、超细碳粉为原料,采用高温碳热还原方法合成出性能良好的β-SiC晶须。运用XRD,SEM,TEM,EDAX等分析检测技术研究了该晶须的结晶特征及生长机理。结果表明:晶须沿<111>方向具有平行的堆垛层错,横断面呈正三角形,晶须顶端存在螺旋位错。该方法生产的β-SiC晶须,其生长过程为“VS”机理。     

铁矿石尾矿合成碳化硅粉末

以铁矿石尾矿和碳黑为原料,采用碳热还原法合成了SiC粉末.用X射线衍射法测定了产物相组成及相对含量.研究了合成温度和恒温时间对反应过程的影响.结果表明:合成温度对SiC粉末的合成过程影响显著,随着合成温度的升高,产物中SiC含量增大,1 480 ℃时,SiC的相对含量达到最大值(82%左右).较长的恒温时间可使还原反应进行得更充分,恒温8 h的样品中SiC的相对含量最高(85%左右).     

温度对碳热还原合成SiC晶须的影响

以工业硅溶胶和碳黑为主要原料,用溶胶-凝胶和碳热还原法进行了合成SiC晶须的试验,探讨了合成温度对产物组成微观形貌的影响.结果表明:合成SiC晶须适合的温度为1600℃,在此条件下得到的产物中SiC晶须含量最高(74%以上)、质量最好.     

Si3N4/SiC/环氧树脂纳米导热复合材料的制备

以硅烷偶联剂KH-560改性的微米氮化硅/纳米碳化硅晶须(Si3N4/SiCw)为导热填料,浇注制备Si3N4/SiC/环氧树脂纳米导热复合材料.研究了环氧树脂种类、Si3N4/SiCw用量、复配比及表面改性对环氧树脂导热、力学和介电性能的影响.结果表明,环氧树脂的热导率随Si3N4/SiCw用量的增加而增大,当改性Si3N4/SiCw用量为50％[m(Si3N4) /m(SiCw)]=3/1时,环氧树脂的热导率为0.98 W/(m· K);复合材料的介电常数随Si3N4/SiCw用量的增加而增大,而力学性能则先增加后降低.     

Mechanical properties and recrystallization of alumina ceramics reinforced by silicon carbide whisker

The mechanical properties and recrystallization of a material consisting of Al₂O₃ and SiC whisker are considered for different hot pressing regimes. The best properties are obtained at an SiC whisker content of 20% in hot pressing in an argon medium at 1600°C (the ultimate bending strength is 600 MPa, the critical coefficient of stress intensityK _Ic=5.5 MPa · m^1/2). The bending strength measured at 1000°C is at least 400 MPa for the material pressed at 1700°C in air. It is established that the presence of SiC whisker on grain boundaries of Al₂O₃ noticeably impedes the growth of alumina grains in recrystallization for all chosen regimes of hot pressing (1650 – 1900°C, 15 – 45 min). The dominant grain size is 1 –5 µm. A mathematical model is suggested for evaluating the maximum grain size in uniform grain growth, which isD*=0.571 [1++(1+16.151/f)^1/2]d, whered, f are the diameter and the volume fraction of SiC whisker. The material can be recommended for use under conditions of thermomechanical stress and abrasive wear.Translated from Ogneupory, No. 5, pp. 8 – 12, May, 1995.     

Processing and fracture behaviour of hot pressed silicon carbide whisker reinforced alumina

The improvement of mechanical properties of silicon carbide whisker reinforced alumina has been investigated with emphasis on the effects of the whisker type and content, the hot pressing temperature and the influence of an interfacial film between the whisker and the matrix. The introduction of silicon carbide whiskers significantly improves the fracture toughness, flexural strength and creep resistance of polycrystalline alumina.

However, these properties are strongly dependent on the size and morphology of whiskers. Large diameter whiskers generate extensive micro-cracking which leads to a decrease in flexural strength. Also, the presence of carbon-coated SiC whiskers substantially increases the high temperature strain rate by promoting cavitation. A grain boundary glassy phase introduced by the carbon coating was also detected.     

Detonation synthesis of nanoscale silicon carbide from elemental silicon

Direct reaction of precursors with the products of detonation remains an underexplored area in the ever-growing body of detonation synthesis literature. This study demonstrated the synthesis of silicon carbide during detonation by reaction of elemental silicon with carbon products formed from detonation of RDX/TNT mixtures. Continuum scale simulation of the detonation showed that energy transfer by the detonation wave was completed within 2–9 μs depending on location of measurement within the detonating explosive charge. The simulated environment in the detonation product flow beyond the Chapman-Jouguet condition where pressure approaches 27 GPa and temperatures reach 3300 K was thermodynamically suitable for cubic silicon carbide formation. Carbon and added elemental silicon in the detonation products remained chemically reactive up to 500 ns after the detonation wave passage, which indicated that the carbon-containing products of detonation could participate in silicon carbide synthesis provided sufficient carbon-silicon interaction. Controlled detonation of an RDX/TNT charge loaded with 3.2 wt% elemental silicon conducted in argon environment lead to formation of ～3.1 wt% β-SiC in the condensed detonation products. Other condensed detonation products included primarily amorphous silica and carbon in addition to residual silicon. These results show that the energized detonation products of conventional high explosives can be used as precursors in detonation synthesis of ceramic nanomaterials.     

碳化硅晶须合成工艺的研究

给出了一种低成本、规模化生产碳化硅晶须的方法。以炭黑和二氧化硅微粉为原料，对双重加热法合成碳化硅晶须进行了研究。确定了合成工艺的优化参数：二氧化硅与炭黑质量比为1．5：1，以三氧化二铁为催化剂，用量为二氧化硅原料总质量的2％，合成温度为1250℃，合成时间为1．5h。该工艺条件下可以得到平均直径为0．6μm、平均长度为30μm、生成率达80％的碳化硅晶须。与常规加热相比，双重加热技术具有节能、省时、生成率高的优点。     

Rapid synthesis of nanostructured porous silicon carbide from biogenic silica

Nanostructured silicon carbide (SiC) is an exceptional material with numerous applications, for example, in catalysis, biomedicine, high-performance composites, and sensing. In this study, a fast and scalable method of producing nanostructured SiC from plant materials by magnesiothermic reduction via self-propagating high-temperature synthesis (SHS) route was developed. The produced biogenic material possessed a high surface area above 200 m²/g with a SiC crystallite size below 10 nm, which has not been done previously by SHS. This method enables affordable synthesis of the material plant-based precursors in a reaction that only takes a few seconds, thereby paving a way for nanostructured SiC production in high volumes using renewable resources. The material was also functionalized with carboxylic acid and bisphosphonate moieties, and its use as metal adsorbent in applications such as wastewater remediation was demonstrated.     

Hybrid effect,mechanical properties and enhancement mechanism of oil-well cement stone with multiscale silicon carbide whisker

Cement-based materials typically have a relatively high compressive strength and a relatively low tensile strength. In this paper, multiscale silicon carbide whiskers (SW) were used to improve mechanical properties of oil-well cement stone. The structure and properties of whisker cement stone were analyzed via mechanical testing and cement sheath integrity. The results demonstrated that multiscale SW mixing showed a positive hybrid effect and could effectively improve the compressive strength, the flexural strength, and the splitting tensile strength of oil-well cement stone by 8.96%, 137.44% and 27.96%. The modulus and porosity of the whisker cement stone significantly reduced. The filling effect, whisker pinning, the pullout, and the whisker bridging were regarded as effective mechanisms for the addition of SW when improving the mechanical properties and microstructures of oil-well cement stone.     

Joining of silicon carbide ceramics using a silicon carbide tape

This paper reports the joining of liquid-phase sintered SiC ceramics using a thin SiC tape with the same composition as base SiC material. The base SiC ceramics were fabricated by hot pressing of submicron SiC powders with 4 wt% Al₂O₃–Y₂O₃–MgO additives. The base SiC ceramics were joined by hot-pressing at 1800-1900°C under a pressure of 10 or 20 MPa in an argon atmosphere. The effects of sintering temperature and pressure were examined carefully in terms of microstructure and strength of the joined samples. The flexural strength of the SiC ceramic which was joined at 1850°C under 20 MPa, was 343 ± 53 MPa, higher than the SiC material (289 ± 53 MPa). The joined SiC ceramics showed no residual stress built up near the joining layer, which was evidenced by indentation cracks with almost the same lengths in four directions.     

原料粒度对合成碳化硅的影响研究

以轮胎半焦为碳源,石英砂为硅源,在1520℃下通过碳热还原法制备了碳化硅。采用XRD、SEM和红外光谱仪等对不同原料粒度条件下制备的碳化硅进行了表征,探究了原料粒度对合成碳化硅物相、形貌、粒度和反应程度的影响规律。结果表明：原料粒度对碳化硅的合成反应进行程度及产物碳化硅的物相组成、形貌、粒度均有十分重要的影响。在一定粒度范围内,随着石英砂粒度的减小,碳化硅晶型变完整,且晶须逐渐减少,碳化硅的粒径分布没有明显变化;随着轮胎半焦粒度的增大,产物物相逐渐变为单一,碳化硅的粒径和晶须所占的比例逐渐减小。此外,通过对产物中C/Si 比的测定和存在中间产物SiO的证实,推测出了碳化硅颗粒的生成机理为气-固（VS）反应,而碳化硅晶须的生成机理为气-气（VV）反应。     

Novel synthesis and characterization of silicon carbide nanowires on graphite flakes

Silicon carbide nanowires were synthesized on the surface of graphite by partially reacting with silicon powders in NaF–NaCl based salt at 1150–1400 °C in argon. The effects of temperature and time of heat treatment as well as Si/graphite ratio on synthesis of SiC nanowires were studied. The results showed that the formation of SiC nanowires started at about 1200 °C, and the amounts of SiC nanowires increased in the resultant powders with increasing temperature. Their morphologies were characterized by scanning electron microscopy and high-resolution transmission electron microscopy. It was found that β-SiC nanowires with diameter of 10–50 nm and various lengths grew along their preferred direction perpendicular to (111). The zeta potential of graphite was also increased after coating with silicon carbide nanowires. SiC nanowires that formed on the graphite surface acted as an anti-oxidant to a certain extent, and they protected the inner graphite from oxidation.