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  • 1
    Electronic Resource
    Electronic Resource
    [s.l.] : Nature Publishing Group
    Nature 374 (1995), S. 526-528 
    ISSN: 1476-4687
    Source: Nature Archives 1869 - 2009
    Topics: Biology , Chemistry and Pharmacology , Medicine , Natural Sciences in General , Physics
    Notes: [Auszug] ADVANCED ceramic materials that can withstand high temperatures (over 1,500 °C) without degradation or oxidation are needed for applications such as structural parts for motor engines, gas turbines, catalytic heat exchangers and combustion systems1,2. Hard, ...
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  • 2
    Electronic Resource
    Electronic Resource
    Westerville, Ohio : American Ceramics Society
    ISSN: 1551-2916
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: The grain-boundary structure of a model SiAlON polycrystal with nominal composition Si5AlON7 was characterized by transmission electron microscopy (TEM) both in an equilibrium (as-processed) state at room temperature and after quenching from elevated temperature. In addition, low-frequency (1–13 Hz) internal friction data were recorded as a function of temperature, showing a pronounced grain-boundary sliding peak positioned at 1030°C. High-resolution transmission electron microscopy (HRTEM) of the equilibrated low-temperature microstructure revealed residual glass only at multigrain junctions, but no amorphous intergranular films were observed. The detection of clean interfaces in the as-processed sample contradicts the internal friction data, which instead suggests the presence of a low-viscosity grain boundary phase, sliding at elevated temperatures. Therefore, a thin section of the as-sintered material was heated to 1380°C and rapidly quenched. HRTEM analysis of this sample showed, apart from residual glass pockets, wetted grain boundaries, which is in line with the internal friction experiment. This wetting-dewetting phenomenon observed in z= 1 SiAlON is expected to have a strong impact not only on high-temperature engineering ceramics but also on geological, temperature-activated processes such as volcanic eruptions.
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  • 3
    ISSN: 1551-2916
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: The oxidation kinetics of amorphous silicon carbonitride (SiCN) was measured at 1350°C in ambient air. Two types of specimens were studied: one in the form of thin disks, the other as a powder. Both specimens contained open nanoscale porosity. The disk specimens exhibited weight gain that saturated exponentially with time, analogous to the oxidation behavior of reaction-bonded Si3N4. The saturation value of the weight gain increased linearly with specimen volume, suggesting the nanoscale pore surfaces oxidized uniformly throughout the specimen. This interpretation was confirmed by high-resolution electron microscopy and secondary ion mass spectroscopy. Experiments with the powders (having a particle size much larger than the scale of the nanopores) were also consistent with measurements of the disks. However, the powder specimens, having a high surface-to-volume ratio, continued to show measurable weight gain due to oxidation of the exterior surface. The wide range of values for the surface-to-volume ratio, which included all specimens, permitted a separation of the rate of oxidation of the free surface and the oxidation of the internal surfaces of the nanopores. Surface oxidation data were used to obtain the rate constant for parabolic growth of the oxidation scale. The values for the rate constant obtained for SiCN lay at the lower end of the spectrum of oxidation rates reported in the literature for several Si3N4 and SiC materials. Convergence in the behavior of SiCN and CVD-SiC is ascribed to the purity of both materials. Conversely, it is proposed that the high rates of oxidation of sintered polycrystalline silicon carbides and nitrides, as well as the high degree of variability of these rates, might be related to the impurities introduced by the sintering aids.
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  • 4
    ISSN: 1551-2916
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: SiCO glasses prepared from sol–gel precursors via pyrolysis in argon at temperatures ranging from 1000° to 1400°C were studied by transmission electron microscopy (TEM), in conjunction with electron energy-loss spectroscopy (EELS). EELS analysis showed that stoichiometric SiCO glass underwent phase separation, forming SiO2- and SiC-based environments. This process started at ∼1200°C. However, at temperatures 〉1300°C, precipitation of nanometer-sized SiC particles embedded in vitreous SiO2 was monitored by high-resolution TEM.
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  • 5
    ISSN: 1551-2916
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Internal friction experiments were conducted on a model SiC polycrystal prepared from preoxidized (high-purity) SiC powder. This material contained high-purity SiO2 glass at grain boundaries in addition to a free-carbon phase, which was completely removed upon powder preoxidation. Comparative tests were conducted on a SiC polycrystal, obtained from the as-received SiC powder with the addition of 2.5 vol% of high-purity SiO2. This latter SiC material was also investigated after annealing at 1900°C for 3 h in a nitrogen atmosphere. Electron microscopy observations revealed a glass-wetted interface structure in SiC polycrystals prepared from both as-received and preoxidized powders. However, the former material also showed a large fraction of interfaces coated by turbostratic graphite. Upon high-temperature annealing in nitrogen, partial glass dewetting occurred, and voids were systematically observed at multigrain junctions. The actual presence of nitrogen could only be detected in a limited number of wetted interfaces. A common feature in the internal friction behavior of the preoxidized, SiO2-added and nitrogen-annealed SiC was a relaxation peak that resulted from grain-boundary sliding. Frequency-shift analysis revealed markedly different characteristics for this peak: both the magnitude of the intergranular glass viscosity and the activation energy for grain-boundary viscous flow were much higher in the nitrogen-annealed material. Results of torsional creep tests were consistent with these findings, with nitrogen-annealed SiC being the most creep resistant among the tested materials.
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  • 6
    ISSN: 1551-2916
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Three high-purity SiAlON materials (Si6−zAlzOzN8−z, z= 1, 2, 3) were characterized with respect to both structure and viscous behavior of internal grain boundaries. Internal friction experiments provided a direct measure of the intrinsic viscosity of grain boundaries and concurrently revealed the occurrence of a grain-boundary interlocking mechanism that suppressed sliding. A residual glass phase (consisting of aluminum-rich SiO2) and nanometer-sized mullite residues were found at glassy triple-grain junctions of the z= 1 SiAlON. A low-melting intergranular phase dominated the high-temperature behavior of this material and caused grain-boundary sliding at temperatures as low as 1100°C. A quantitative analysis of the grain-boundary internal friction peak as a function of oscillation frequency indicated an intergranular film viscosity of log η∼ 7.5 Pa · s at 1100°C. Glass-free grain boundaries were a characteristic of SiAlON materials with z≥ 2, which yielded a significant improvement in refractoriness as compared to the z= 1 SiAlON material. In these materials, relaxation resulting from grain-boundary sliding was suppressed, and the internal friction curve simply experienced an exponential-like increase.
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  • 7
    ISSN: 1551-2916
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Monolithic polymer-derived Si-C-N ceramics were processed by blending an oligomeric Si-C-N precursor (liquid polysilazane) with 70 vol% of crosslinked or pyrolyzed Si-C-N powder particles, which were obtained from the same liquid precursor preheated at 300° or 1000°C, respectively. Powder compacts subsequently were annealed at 300°C to crosslink the liquid precursor acting as a binder between the powder particles, thus yielding monolithic green bodies. Heat treatment at 1540°C was performed to initiate crystallization in the various samples. Microstructure development and, in particular, crystallization behavior were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and preliminary nuclear magnetic resonance (NMR) spectroscopy. The material containing 300°C polymer powder (with oligomeric binder, also crosslinked at 300°C) revealed a homogeneous amorphous microstructure after exposure to temperatures of 1540°C. In contrast, the specimen containing powder particles preheated at 1000°C exhibited a high volume fraction of SiC crystallites within regions that were previously filled by the binder; however, the Si-C-N powder particles themselves remained amorphous. SEM observations as well as XRD studies showed the formation of idiomorphic SiC and Si3N4 crystallites on specimen surfaces as well as along internal crack walls. This finding suggested that vapor-phase reactions at the surface were involved in the formation of crystalline phases at temperatures 〉1250°C. Moreover, NMR spectroscopy data indicated a phase separation process, implying structural rearrangement prior to crystallization.
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  • 8
    Electronic Resource
    Electronic Resource
    Westerville, Ohio : American Ceramics Society
    ISSN: 1551-2916
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Monolithic mullite with low sintering shrinkage was synthesized from polymer/filler blendsMthat is, siloxane/alumina (siloxane/Al2O3) (and siloxane/aluminum (siloxane/Al)) mixtures. The synthesis was based on a reaction-bonding process of amorphous silica, which formed when the siloxane was oxidized, with Al2O3 (or oxidized aluminum filler) at temperatures 〉1250°C. Thermodynamic calculations were used to calculate the phase composition at equilibrium. Thermoanalytical, infrared-spectroscopic, and microscopic techniques were applied to reveal the microstructural evolution. The corresponding volume changes were used to evaluate the linear shrinkage, based on the quantitative phase assemblage.
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  • 9
    ISSN: 1551-2916
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Silicon nitride materials that contained different mixtures of sintering aids were investigated with respect to microstructure development and resulting fracture toughness. Postsintering annealing at 1850°C for various times was adopted in order to coarsen the respective microstructures. Although constant processing conditions were used, a marked variation in fracture toughness of the Si3N4 materials was evaluated. With a larger grain diameter of the Si3N4 grains, an increase in fracture resistance was generally observed. However, a correlation between fracture toughness and apparent aspect ratio could not be established. The observed changes in microstructure were in fact caused by the difference in secondary-phase chemistry. Si3N4 grain growth was dominated by diffusion-controlled Ostwald ripening and was hence affected by the viscosity of the liquid at processing temperature. In addition, crystallization at triple pockets also depends on the sintering additives employed and was found to influence fracture toughness by altering the crack-propagation mode as a consequence of local residual microstresses at grain boundaries. The stress character (compressive vs tensile) is governed by the type of crystalline secondary phase formed. Moreover, a variation in interface chemistry changes the glass network structure on the atomic level, which can promote transgranular fracture, i.e., can result in a low fracture resistance even in the presence of favorable large Si3N4 matrix grains. Therefore, secondary-phase chemistry plays a dominant role with respect to the mechanical behavior of liquid-phase-sintered Si3N4. Fracture toughness is, in particular, influenced by (i) altering the residual glass network structure, (ii) affecting the secondary-phase crystallization at triple pockets, and (iii) changing the Si3N4 grain size/morphology by affecting the diffusion rate in the liquid. The first two effects of secondary-phase chemistry are superimposed on the merely structural parameters such as grain diameter and apparent aspect ratio.
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  • 10
    ISSN: 1551-2916
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: The excess carbon of various polysilazane precursors with varying carbon contents was investigated using 13C MAS NMR, Raman and ESR spectroscopies, and microwave conductivity measurements. Microstructure characterization was investigated using TEM. The collected data were compared with those from a previous study on the same precursor. This study focused on the distribution and appearance of the free-carbon phase. Although the spectroscopic techniques showed no differences in the structure of the free-carbon phase, a clear distinction between the various precursors was found using microwave conductivity and high-resolution TEM imaging.
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