化学激励燃烧合成Si3N4/SiC复合粉体的研究

研究了利用聚四氟乙烯作活化剂时Si／C混合粉末在氮气中燃烧合成Si3N4／SiC复合粉体。结果表明：当聚四氟乙烯的加入量为10％(质量分数)时可有效激励Si-C弱放热反应，使之以燃烧合成方式生成Si3N4／SiC复相粉。在埋粉条件下Si／C／SiC混合粉末也可以实现燃烧合成Si3N4／SiC复相粉。氮气参与反应时可进一步提高燃烧反应温度，并且首先以气相-晶体生长机制生成Si3N4，然后在高温贫氮的反应前沿Si3N4分解，再与C反应生成SiC。在Si3N4／SiC复合粉中Si3N,形貌以晶须为主。综合X射线衍射分析、扫描电镜观察及原子力显微镜观察对实验结果进行了讨论，解释了Si3N4晶须的形成原理。     

NiO催化氮化制备Si_3N_4/SiC复合材料及其高温性能

以原位生成的NiO纳米颗粒为催化剂,采用催化氮化的方法制备Si3N4/SiC复合材料,研究了所制备复合材料的常温物理性能、高温力学性能、抗热震性、抗氧化及抗冰晶石侵蚀性能。结果表明:1)所制备Si3N4/SiC复合材料的常温耐压强度及抗折强度值分别为131.0及24.6MPa;2)Si3N4/SiC复合材料的高温抗折强度随着温度的升高而增加,1573K时达到最大值后又缓慢下降,但即使1673K时复合材料的高温抗折强度仍高于其常温抗折强度;3)Si3N4/SiC复合材料具有较好的抗热震性能,当实验温度为1573K,采用水冷时,其强度保持率仍有50%左右;4)所制备Si3N4/SiC复合材料开始氧化温度约为1173K,其抗氧化性能优于无催化剂时制备的Si3N4/SiC复合材料;5)所制备的复合材料具有良好的抗冰晶石侵蚀性能。由于NiO纳米颗粒催化生成大量的Si3N4晶须,这些晶须交互分布在骨料之间,形成网络状结构,从而提高了复合材料的性能。     

NiO催化氮化制备Si_3N_4/SiC复合材料及其高温性能

以原位生成的NiO纳米颗粒为催化剂,采用催化氮化的方法制备Si3N4/SiC复合材料,研究了所制备复合材料的常温物理性能、高温力学性能、抗热震性、抗氧化及抗冰晶石侵蚀性能。结果表明:1)所制备Si3N4/SiC复合材料的常温耐压强度及抗折强度值分别为131.0及24.6MPa;2)Si3N4/SiC复合材料的高温抗折强度随着温度的升高而增加,1573K时达到最大值后又缓慢下降,但即使1673K时复合材料的高温抗折强度仍高于其常温抗折强度;3)Si3N4/SiC复合材料具有较好的抗热震性能,当实验温度为1573K,采用水冷时,其强度保持率仍有50%左右;4)所制备Si3N4/SiC复合材料开始氧化温度约为1173K,其抗氧化性能优于无催化剂时制备的Si3N4/SiC复合材料;5)所制备的复合材料具有良好的抗冰晶石侵蚀性能。由于NiO纳米颗粒催化生成大量的Si3N4晶须,这些晶须交互分布在骨料之间,形成网络状结构,从而提高了复合材料的性能。     

NiO催化氮化制备Si_3N_4/SiC复合材料及其高温性能

以原位生成的NiO纳米颗粒为催化剂,采用催化氮化的方法制备Si3N4/SiC复合材料,研究了所制备复合材料的常温物理性能、高温力学性能、抗热震性、抗氧化及抗冰晶石侵蚀性能。结果表明:1)所制备Si3N4/SiC复合材料的常温耐压强度及抗折强度值分别为131.0及24.6MPa;2)Si3N4/SiC复合材料的高温抗折强度随着温度的升高而增加,1573K时达到最大值后又缓慢下降,但即使1673K时复合材料的高温抗折强度仍高于其常温抗折强度;3)Si3N4/SiC复合材料具有较好的抗热震性能,当实验温度为1573K,采用水冷时,其强度保持率仍有50%左右;4)所制备Si3N4/SiC复合材料开始氧化温度约为1173K,其抗氧化性能优于无催化剂时制备的Si3N4/SiC复合材料;5)所制备的复合材料具有良好的抗冰晶石侵蚀性能。由于NiO纳米颗粒催化生成大量的Si3N4晶须,这些晶须交互分布在骨料之间,形成网络状结构,从而提高了复合材料的性能。     

燃烧合成制备Si3N4-TiN-SiC陶瓷的显微结构

以TiSi2为反应原料,SiC作稀释剂,燃烧合成制备Si3N4-TiN-SiC陶瓷.利用燃烧波"淬熄"法使反应各个阶段的物相得以保留,通过X射线衍射及扫描电镜分析TiSi2在燃烧合成中的反应过程及显微组织转化.结果表明:完全反应后产物的主相为Si3N4,其余为TiN和SiC.在燃烧过程中,TiSi2首先受热熔化,包覆于SiC颗粒表面,随后与N2反应生成TiN和Si.Si在高热作用下发生熔化、汽化,液态Si与未反应的TiSi2互溶.生成的Si与氮气发生反应,形成Si3N4晶核,并不断长大.燃烧合成反应过程中,Si3N4晶须的生长十分复杂,由气-液-固机制、气-固机制及蒸发凝聚的气相生长机制共同作用.     

逆反应烧结制备碳化硅/氮化硅复合材料的工艺

制备Si3N4／SiC复合材料的常规反应烧结是以Si和SiC为原料进行氮化烧结,而逆反应烧结是以Si3N4和SiC为原料,首先使Si3N4反向反应为活性氧化物后再进行烧结。建立逆反应烧结工艺制备Si3N4／SiC复合材料的热力学基础。确定了Si3N4先于SiC氧化;氧化产物可以是SiO2,也可以是Si2N2O;形成的SiO2氧化膜不会与基体材料反应;在膜与基体之间可能生成Si2N2O。论证了逆反应烧结的热力学可行性。通过6个烧结实验,证实了其热力学分析的正确性,并从工艺参数与密度变化、残氮率和比强度等关系筛选出最佳的烧结工艺参数。     

氮化烧结制备Si3 N4 -SiC复相陶瓷

以酚醛树脂作为结合剂,以冷等静压方法成型制备氮化烧结Si3N4-SiC复相陶瓷,研究了结合剂对坯体强度和生成材料物相组成的影响。坯体强度随酚醛树脂含量增加而提高,最高强度达到23MPa,实现坯体可直接机械加工。经过氮化烧结,生成材料物相中含有SiC,含量达到7.1%～15.7%,并观察到细小的等轴颗粒αSi3N4、棒状晶粒βSi3N4以及少量针状和晶须状Si3N4。SiC颗粒与Si3N4结合在一起,被Si3N4包裹。Si3N4-SiC复相材料的生成机理:300～600℃,酚醛树脂发生裂解,形成单质C,残碳率为50%;1000～1100℃,C开始与Si发生固相反应,形成SiC;1100℃后,Si开始发生氮化反应,生成Si3N4。     

通过氮化硅基质中SiO2的现场碳热还原反应制备Si3N4-SiC微／纳米复合材料

利用α-Si3N4、无定形碳(炭黑)和Y2O3组成的混合物，通过对Si3N4基质微粒表面上的SiO2进行碳热还原反应，或在原料基质中加入该混合物，制备了SiC／Si3N4微／纳米复合材料。进行特殊的热处理后，CO气体(碳热还原反应产物)从材料中排出，材料残余孔隙度降至2％以下。在SiC和Si3N4界面上，存在包含无定形富氧层的粒间和粒内SiC内含物，它是由单体碳和熔融二氧化硅反应而生成的。反应要消耗晶界相中的二氧化硅。晶界化学性质的改变对本纳米级复合材料的室温性能和高温性能都有影响。     

Si_3N_4-Al_2O_3系陶瓷材料表面氧化层的XPS分析

Si2N4陶瓷材料具有高强度、耐磨、耐高温、耐热冲击和有自润滑性等特点，因此可作为高温结构材料。然而，Si3N4陶瓷材料在高温下使用时往往存在着氧化问题，这直接影响了Si3N4陶瓷材料的使用寿命和各种性能。对其氧化层中的方石英相大多是用X射线衍射分析（XRD）的方法来测定的。为了更好的研究Si3N4陶瓷材料表面氧化层的组成，在采用X射线衍射分析方法的同时，还采用XPS分析方法对表面氧化层中Si的存在状态进行了分析。首先对在空气中1300℃下氧化了100h的Si3N4陶瓷材料表面的氧化层进行了XPS分析，结果表明在表面氧化层中存在的…     

梭式氮化窑用Si_3N_4-SiC匣钵砖用后分析

利用XRD、SEM和EDAX对在梭式氮化窑中使用1年后的反应烧结Si3N4-SiC匣钵砖内外侧进行了分析。结果表明:在匣钵外侧(氧化气氛),匣钵砖表面12 mm厚的区域呈完全氧化状态,主要氧化产物是SiO2;紧随其后的12～20 mm区域呈部分氧化状态,氧化产物主要为Si2N2O及少量SiO2;20 mm以后区域无明显氧化特征。在匣钵内侧(氮气气氛),匣钵砖表面出现了约0.2 mm厚的氧化层,主要氧化产物是SiO2,该SiO2可能是由气态SiO氧化形成的,而气态SiO主要来自SiC的氧化及氮化过程中形成的气态SiO;从显微结构可以看出,SiC颗粒表面氧化明显。     

Fabrication and optimization of a clay-bonded SiC flat tubular membrane support for microfiltration applications

SiC has excellent structural and mechanical properties and also has excellent properties related to membrane performance. High processing temperature increases the costs of SiC products and thus limits their use. In this study, we fabricated SiC-based ceramic support layers using a clay-bonding technique. Kaolin, a well-known clay, was used as a binder for silicon-carbide particles. Three different SiC powders were used on the basis of particle size for fabrication by the extrusion method, which converts powders into flat tubular form. The resultant supports are sintered at 1300–1500 °C in air and evaluated for their structural properties, pore characteristics and permeability. It is evident from the study that we can produce a support layer with small-sized SiC powder that has a high open porosity and high strength with a smaller pore size and lower permeability in comparison with layers produced with a large-sized starting SiC powder. Additionally, the produced support layer could be used as a stand-alone membrane for 1 µm particles.     

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。     

Zrc ceramics incorporated with different-sized SiC particles

ABSTRACT

Three different SiC powders with average particle sizes of 0.45, 3.5 and 10?µm were used to prepare ZrC-20vol.-% SiC ceramics by hot pressing. The effects of SiC particle size on the densification, microstructure, mechanical properties and thermal properties of ZrC–SiC ceramics were studied. Ceramics prepared from SiC with finer particle sizes exert higher bending strength, hardness and lower thermal conductivity. The ZrC–SiC ceramics with a starting SiC particle size of 3.5?µm has relative high fracture toughness than others. Analysis indicates that SiC grain size and the grain boundaries control the thermal conductivity ZrC–SiC ceramics. Ceramics prepared from SiC with the particle size of 10?µm exhibits the highest thermal conductivity due to the larger grains and less grain boundaries.     

Effect of SiC Particles on Mechanical Properties of Laminated (SiCw+SiCp)/SiC Ceramic Composites

Laminated (SiC_w+SiC_p)/SiC ceramic composites were fabricated by tape casting and chemical vapor infiltration (CVI), and the effect of SiC particles on strengthening/toughening of the composites was investigated. When the SiC particle content was constant, the mechanical properties of (SiC_w+SiC_p)/SiC composites were increased with increasing SiC whisker content. When the SiC particle content was varied, the mechanical properties of (SiC_w+SiC_p)/SiC composites were dependent on SiC particle content. The addition of SiC particles can increase the strength of the matrix and the crack propagation resistance, the former increased the strength and the latter increased the toughness.     

Factors that influence the flexural strength of SiC-based porous ceramics used for hot gas filter support

The influences of molding pressures, bonding phase contents, and SiC particle sizes on the flexural strength of SiC-based porous ceramics were investigated based on their microstructure of fracture surface. The SEM morphologies and EDS element analysis results of fracture surface showed that there were two different kinds of fracture points: SiC particle fracture points and bonding phase fracture points. It is found that molding pressures, bonding phase contents, and SiC particle sizes affect the SiC particle fracture point area in the fracture surface, and the fraction of the SiC particle fracture point area in the minimum solid area of fracture surface is a determined influence factor for the flexural strength of SiC-based porous ceramics used for hot gas filter support.     

Influence of silicon carbide particle size on the microstructure and mechanical properties of zirconium diboride–silicon carbide ceramics

The influence of silicon carbide (SiC) particle size on the microstructure and mechanical properties of zirconium diboride–silicon carbide (ZrB₂–SiC) ceramics was investigated. ZrB₂-based ceramics containing 30 vol.% SiC particles were prepared from four different α-SiC precursor powders with average particle sizes ranging from 0.45 to 10 μm. Examination of the dense ceramics showed that smaller starting SiC particle sizes led to improved densification, finer grain sizes, and higher strength. For example, ceramics prepared from SiC with the particle size of 10 μm had a strength of 389 MPa, but the strength increased to 909 MPa for ceramics prepared from SiC with a starting particle size of 0.45 μm. Analysis indicates that SiC particle size controls the strength of ZrB₂–SiC.     

Self-Crack-Healing Behavior of Mullite/SiC Particle/SiC Whisker Multi-Composites and Potential Use for Ceramic Springs

To improve fracture toughness and encourage excellent self-crack-healing ability, mullite/SiC particle/SiC whisker multi-composites and mullite/SiC whisker composites were hot pressed. The crack-healing abilities and mechanical properties of these sintered composites were investigated. Based on the obtained results, the usefulness of the mullite composite as a material for springs was discussed. The part of mullite/15 vol% SiC whisker/SiC 10 vol% particle containing healed cracks retained high reliability over the whole measured temperature range. When the crack-healing ability was endowed by SiC whiskers alone, the parts containing the healed pre-cracks were found to have a heat-resistance limit temperature. Mullite/15 vol% SiC whisker/10 vol% SiC particle multi-composite had the best potential as a material for springs used at high temperatures, because it had an adequate crack-healing ability as well as shear deformation ability almost two times stronger than that of monolithic mullite.     

Preparing SiC/diamond coatings via chemical vapor deposition of SiC on diamond-coated graphite and their frictional properties

SiC/diamond coatings with excellent frictional properties were successfully prepared using graphite as substrate. Diamond particles with size of 25–38 μm were firstly bonded on graphite substrate through PVA glue, followed by chemical vapor deposition (CVD) of SiC with varied MTS flow on the diamond-coated graphite substrate to enhance the adhesion of diamond particles. The influence of the MTS flow on the SiC coatings was investigated. The results showed that polycrystalline SiC coating with good crystallinity has been obtained. With MTS flow increasing, the SiC grains feature increased surface roughness and greater sizes of the SiC crystallite resulting from the co-deposition of SiC and carbon with increased carbon containing species. Reciprocating sliding wear tests were conducted to investigate the coefficient of friction. With increasing applied load, while the low-flow specimens showed a remarkable increase in the friction coefficient resulting from degradation of the SiC coatings, the high-flow specimens maintained a relatively low friction coefficient during wear tests indicating strong holding force to diamond particles of the SiC coatings. The reason for low friction coefficient of the high-flow specimens was that GCr15 steel ball was wearing by the SiC/diamond coatings with good affinity to the substrate resulting in a flat–flat contact on the contact area.     

Flexural Creep Deformation of ZrB2/SiC Ceramics in Oxidizing Atmosphere

Flexural creep of ZrB₂/0–50 vol% SiC ceramics was characterized in oxidizing atmosphere as a function of temperature (1200°–1500°C), stress (30–180 MPa), and SiC particle size (2 and 10 μm). Creep behavior showed strong dependence on SiC content and particle size, temperature and stress. The rate of creep increased with increasing SiC content, temperature, and stress and with decreasing SiC particle size, especially, at temperatures above 1300°C. The activation energy of creep showed linear dependence on the SiC content increasing from about 130 to 511 kJ/mol for ceramics containing 0 and 50 vol% 2-μm SiC, respectively. The stress exponent was about 2 for ZrB₂ containing 50 vol% SiC regardless of SiC particle size, which is an indication that the leading mechanism of creep for this composition is sliding of grain boundaries. Compared with that, the stress exponent is about 1 for ZrB₂ containing 0–25vol% SiC, which is an indication that diffusional creep has a significant contribution to the mechanism of creep for these compositions. Cracking and grain shifting were observed on the tensile side of the samples containing 25 and 50 vol% SiC. Cracks propagate through the SiC phase confirming the assumption that grain-boundary sliding of the SiC grains is the controlling creep mechanism in the ceramics containing 50 vol% SiC. The presence of stress, both compressive and tensile, in the samples enhanced oxidation.     

Influence of annealing on the mechanical properties of SiC–Si composites with sub-micron SiC microstructures

The influence of annealing temperature (1000, 1100 and 1200°C) on the mechanical properties of SiC–Si composites has been evaluated. Three SiC powders with particle sizes in the range of 0.24 to 0.7 μm were used to produce the composites. Before application the SiC powders were treated with hydrofluoric acid to remove the extent of SiO₂. With this treatment a successful infiltration of green-bodies especially produced of SiC powder with a mean particle size of 0.24 μm was possible. The bending strength decreased with decreasing SiC starting particle size as well as with increasing annealing temperature. However, the fracture toughness was independent on SiC starting particle size and annealing temperature. XRD diffraction analysis showed that internal stress, expressed by broadening of XRD peaks, is low and had no effects on the mechanical properties of the composites.