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  • 1
    ISSN: 0268-2605
    Keywords: precursor ; ceramic ; thermolysis ; silicon ; carbodi-imide ; boron ; hydroboration ; plastic forming ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis, by two different reaction pathways, of boron-modified polysilylcarbodi-imides of general type {B[C2H4Si(R)NCN]3}n (R =­singly bonded organic ligand) and the plastic-forming and the thermal behavior of these polymers are described. Compounds {B[C2H4Si(R)NCN]3}n [2a, R = H; 2b, R = CH3; 2c, R = (NCN)0.5] can be obtained by treatment of the vinyl-substituted polysilylcarbodi-imides [(H2C=CH)(R)SiNCN]n [1a, R = H; 1b, R = CH3; 1c, R = (NCN)0.5] with borane dimethylsulfide BH3·S(CH3)2. The polysilylcarbodi-imides 1a-1c themselves are accessible via the reaction of vinyl-substituted chlorosilanes (H2C=CH)-­(R)SiCl2 with cyanamide H2N-C≡N in the presence of pyridine or by a non-oxide sol-gel process of vinylated chlorosilanes and bis(trimethylsilyl)carbodi-imide, (H3C)3SiN=C=NSi(CH3)3. In the second method for the synthesis of 2a-2c, hydroboration of vinyl-substituted chlorosilanes (H2C=CH)(R)SiCl2 with borane dimethylsulfide, borane trimethylamide or borane triethylamide to yield the tris[(chlorosilyl)ethyl]boranes B[C2H4Si(R)Cl2]3 (3a, R = H; 3b, R = CH3; 3c, R = Cl) is followed by treatment of the as-obtained compounds with bis(trimethylsilyl)carbodi-imide, which results in the formation of the hydroborated polysilylcarbodi-imides 2a-2c. The thermogravimetric behavior of the polymers 1a-1c and 2a-2c up to 2300°C is reported. It is shown that boron-modified polysilylcarbodi-imides are suitable precursors for the preparation of dense bulk ceramics. Therefore, the preparation of green bodies of the hydroborated polysilylcarbodi-imides 2a-2c by plastic forming (PF) is described. A series of experiments points to the fact that the microstructure of the as-obtained ceramic monoliths obtained by subsequent thermolysis of the plastic-formed green bodies is strongly influenced by the conditions during plastic forming. © 1998 John Wiley & Sons, Ltd.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1662-0356
    Source: Scientific.Net: Materials Science & Technology / Trans Tech Publications Archiv 1984-2008
    Topics: Natural Sciences in General , Technology
    Notes: Boron-modified polyvinylsilazanes have been studied for suitability as fiber precursor. Amelt-tractable polymer displaying Si- and N-bonded methyl groups was successfully processed intogreen fibers ~18μm in diameter via a melt-spinning process. After the shaping process, the use ofan ammonia curing atmosphere at 200°C allowed to increase the ceramic yield of the polymer, thenavoid inter-fiber fusion during the further increase of the temperature. As-cured fibers wereannealed in the temperature range 1000-1800°C in a nitrogen atmosphere to provide SiBCNceramic fibers black colored, of flexible form and ~12μm in diameter in different crystallinity statesgoing from totally amorphous below 1600°C to well-crystallized at 1800°C. The excellent strengthretention after heat-treatment at 1600°C (1.3-1.5GPa) is clearly related to the high amorphousstability of fibers. Elemental compositions of such amorphous fibers showed a typical chemicalformula of Si3.0B1.0C5.0N2.4. Between 1600°C and 1700°C, the fiber strength decreased to 0.9GPathen dropped to about one-quarter the original value at 1800°C while structural changes wereevident by XRD analysis
    Type of Medium: Electronic Resource
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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: Surface oxidation occurred during pyrolysis of SiC particulate-reinforced composites (PRCs) with a precursor-derived Si–C–N matrix. In contrast, such an oxidation was not observed in pure Si–C–N ceramics. The present investigation discusses the possible reasons for this, and reports on the influence of such an oxidation on the microstructure and the mechanical and thermal properties of PRCs by the precursor-impregnation and pyrolysis method. The high-temperature mass stability of the PRCs in Ar deteriorated owing to the decomposition of SiO2 formed by oxidation. The effects of the pyrolysis schedule on the processing and mechanical properties of PRCs are also investigated.
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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: The characterization of Si-B-C-N amorphous ceramics using isothermal compression creep testing in the temperature range of 1200°–1500°C is reported. The deformation rate contains a stress-dependent component that is proportional to the applied stress, which indicates that this portion of the deformation mechanism is based on viscous flow. An increase in the creep resistance is observed, following either preliminary annealing or hot isostatic pressing, which may be explained by a reduction of free volume in the amorphous material. The application of two deformation models that are used to predict similar deformation behavior in metallic glasses also is discussed. Although both models accurately predict the time dependence of the deformation rate of precursor-derived amorphous ceramics, the free-volume model fits the observed temperature dependence better than the “two-step” rearrangement model.
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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: Amorphous Si-B-C-N ceramic powder samples obtained by thermolysis of boron-modified polysilazane, {B[C2H4Si(H)NH]3}n, were isothermally annealed at different temperatures (1400–1800°C) and hold times (3, 10, 30, and 100 h). A qualitative and semiquantitative analysis of the crystallization behavior of the materials was performed using X-ray diffraction (XRD). The phase evolution was additionally followed by 11B and 29Si MAS NMR as well as by FT-IR spectroscopy in transmission and diffuse reflection (DRIFTS) modes. Bulk chemical analyses of selected samples were performed to determine changes in the chemistry/phase composition of the materials. It was observed that silicon carbide is the first phase to nucleate around 1400–1500°C, whereas silicon nitride nucleates at and above 1700°C. Crystallization accelerates with increasing annealing temperature and proceeds with increasing annealing time. Furthermore, the surface area of the powders strongly influences the thermal stability of silicon nitride and thus controls overall chemical and phase composition of the materials on thermal treatment.
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