Conversion of polyaluminocarbosilane(PACS) to Si-Al-C-(O) fibers:evolutions and effect of oxygen

The evolvement of oxygen from polyaluminocarbosilane(PACS) to Si-Al-C-(O) fibers and its effect on properties were investigated by element analysis, solid-state 27Al nuclear magnetic resonance(NMR), Fourier transform infrared spectroscopy(FT-IR), thermo-gravimetric analyses(TGA), scanning electron microscope(SEM) and X-ray diffraction(XRD). Element analysis of PACS precursor polymer gives an empirical formula of SiC2.1H11.1O0.12Al0.024. 27Al NMR spectra mass gain shows that the oxygen of cured PACS fibers comes from aluminum aletylacetanate (Al(AcAc)3) and the curing process. Oxygen content can be regarded as a constant mass during the pyrolysis process. During the sintering process of Si-Al-C-O fibers into Si-Al-C fibers, oxygen and carbon decreases with the release of a small amount of CO and/or SiO. Oxygen has a positive effect on the ceramic yield while has a negative effect on the crystallization of Si-Al-C-O fibers. It has great influence on mechanical properties of Si-Al-C-O and excellent tensile strength is usually obtained at the oxygen content of 8%-10%. The Si-Al-C-(O) fibers have excellent thermal stability and creep resistance.

Thermal stability and curing kinetics of polycarbosilane fibers

Thermal stability and curing kinetics of polycarbosilane (PCS) fibers were studied by thermogravimetry (TG), Fourier transform infrared spectroscopy(FT-IR). Curing is an essential step in the preparation of SiC fibers and the properties of SiC fibers are affected greatly by curing conditions. TG measurement performed in air shows that mass gain starts at approximately 200℃ and PCS fibers are sensitive to oxygen. Curing with oxygen, which results in crosslinking on the surface, enabled PCS fibers to retain its shape during high-temperature pyrolysis. The curing of PCS fibers is oxidation of Si─H and Si─CH3, then Si─O─Si and Si─O─C bonds are formed. This is a first order reaction, with activation energy of 79.27 kJ/mol, and the pre-exponential factor is calculated as 3.07×106. The kinetics model was obtained and the experimental data of PCS fibers show good agreement with the kinetics model.

Processing and characterization of C_f/SiC composites

Carbon fiber-reinforced SiC composites were prepared by precursor pyrolysis-hot pressing （PP-HP） and precursor impregnation-pyrolysis （PIP）, respectively. The effect of fabrication methods on the microstructure and mechanical properties of the composites was investigated. It was found that the composite prepared by PP-HP exhibits a brittle fracture behavior, which is mainly ascribed to a strongly bonded fiber/matrix interface and the degradation of the fibers caused by a higher processing temperature. On the contrary, the composite prepared by PIP shows a tough fracture behavior, which could be rationalized on the basis of a weakly bonded fiber/matrix interface as well as a higher strength retention of the fibers. As a result, in comparison with the composite prepared by PP-HP, the composite prepared by PIP achieves better mechanical properties with a flexural strength of 573.4 MPa and a fracture toughness of 17.2 MPa.m^1/2.

Photocatalytic properties of TiO_2 bonded active carbon composites prepared by SOL-GEL

Photocatalyst of TiO2 bonded active carbon （TiO2/AC）, was prepared via sol-gel method from a mixture of TiO2 sol with active carbon. Post heat treatment was performed at 250 ℃ for 2 h in air and then kept at 400 ℃ to 600 ℃ under a flow of nitrogen for 2 h. The TiO2/AC composites obtained were characterized by SEM, XRD, UV-vis and BET. The photocatalytic activities of the TiO2/AC composites were studied in comparison with TiO2, AC, P-25 and a mixture of TiO2 and AC, respectively. The Ramnant rate of Rhodamine B absorbed by the active carbon is found to be almost 70% and the remnant rates of the Rhodamine B decolorized by TiO2 and the mixture of TiO2 and the active carbon are 30% and 25%, respectively. However, nearly complete removal of Rhodamine B is observed for a TiO2/AC composite after 200 min under UV irradiation, which will take the P-25 commercial product 5 h. Therefore, the TiO2/AC composite is much more effective in decolorization of aqueous Rhodamine B. In addition, the composite can be easily separated from solutions.

Preparation and characterization of continuous high-temperature resistant Si-Al-C fibers by one-step method

Using polymer-derived technology, continuous high-temperature resistant Si-Al-C fibers were prepared by one step method, which included melt-spinning of polya-luminocarbosilane (PACS), curing of continuous PACS fibers, and sintering of the cured products. The results show that the average diameter and tensile strength of continuous Si-Al-C fibers are 11 to 12 μm and 1.8 to 2.0 GPa, respectively. The chemical formula of Si-Al-C fibers is SiC1.01O0.0400Al0.024, which is nearly stoichometric. The fibers are mainly composed of β-SiC crystalline, small amount of α-SiC, and amorphous SiC. Continuous Si-Al-C fibers exhibit excellent thermal stability. When the fibers were exposed in argon for 1 h, the tensile strength did not decrease until 1500℃. After heat treatment at 1800℃ in argon for 1 h, the fibers maintained about 80% of the initial strength. It was higher than that of Nicalon and Hi-Nicalon fibers.

Synthesis of ceramic precursor polycarbosi-lane (PCS) under supercritical fluids (SCFs) state

Using xylene as supercritical fluids (SCFs) media and polydimethylsilane (PDMS) as raw material, the ceramic precursor polycarbosilane (PCS) with moderate mo-lecular weight and narrow molecular weights distribution was synthesized under high pressure and temperature in autoclave. Softening-point test, Fourier transform infrared spectroscopy (FT-IR), gel permeation chromatography (GPC), element analysis and the yield test of PCS were adopted to characterize the SCFs-method and compared with two other PCS synthesis methods named normal-pressure high-temperature (NP) method and high-pressure hith-temperature (HP) method. The results indicate that the PCS maintains a high Si-H content and its chemical formula is SiC1.91H7.27O0.05. The yield is 63.5 wt% which has been improved by about 20 wt%, the softening-point is 180―220 ℃, the number average molecular weight is 1477 and the molecular weights distribution index is 1.61. The synthesis method via supercritical fluids with good diathermancy and reaction uniformity is a new feasi-ble method of synthesizing PCS with good qualities.