Xujin Bao

Preparation of silicon carbide foams using polymeric precursor solutions

A simple method was developed to produce silicon carbide foams using polysilane polymeric precursors. Polyurethane foams were immersed in polysilane precursor solutions to prepare pre-foams. Subsequently, these were heated in nitrogen at different temperatures in the range of 900°C to 1300°C. The silicon carbide foams produced in this manner showed well-defined open-cell structures and the struts in the foams were free of voids. The shrinkage which accompanies pyrolysis of the pre-foams was reduced with increasing the concentration of the polymeric precursor solutions.

Preparation of silicon carbide–silicon nitride composite foams from pre-ceramic polymers

Abstract A new method of forming silicon carbide–silicon nitride composite foams is presented. These are prepared by immersing a polyurethane foam in a polysilane precursor solution mixed with Si3N4 powder to form a pre-foam followed by heating it in nitrogen at >900°C. X-ray diffraction patterns indicate that a SiC–Si3N4 composite was formed after sintering the ceramic foam at >1500°C. Micrographs show that most of these foams have well-defined open-cell structures and macro-defect free struts. The shrinkage is reduced considerably due to the addition of Si3N4 particles.

Modification of montmorillonite with aminopropylisooctyl polyhedral oligomeric silsequioxane

Sodium montmorillonite (Na-MMT) was modified with various amounts of aminopropylisooctyl polyhedral oligomeric silsequioxane (POSS) and a second surfactant (alkyl ammonium based) via ion-exchange reactions. Interlayer spacing, interlamellar structure, and thermal and surface properties of these organoclays were characterized by wide angle X-ray diffraction, thermogravimetric analysis, and contact angle measurement. The interlayer space of POSS-modified clay (POSS-MMT) was strongly dependent on the arrangement of POSS surfactant but less dependent on the POSS concentration. The sodium ions in Na-MMT were only partially exchanged by protonized POSS due to the steric hindrance effect. In addition, the dual-surfactant-modified clays exhibited increased exchange ratios by controlling the amount of the second surfactant, resulting in a good balance in hydrophobicity and polarity of the modified clays. The resultant organoclays were mixed with polypropylene (PP) via a melt-compounding method. It was found that the dual-surfactant-modified clays with low polarity and similar hydrophobicity to PP were well dispersed in the PP matrix.

Aluminium oxide nanoparticles prepared by water-in-oil microemulsions

A new water-in-oil microemulsion, consisting of the non-ionic surfactant Triton X-114, cyclohexane as the oil phase and 1.0 M AlCl3 aqueous solution as the aqueous phase, was developed and used to synthesise aluminium oxide (Al2O3) nanoparticles. The partial phase diagram of this ternary system was also determined at 38 °C. Syntheses of Al2O3 nanoparticles were carried out in a range of microemulsions with a fixed oil∶surfactant ratio of 70∶30 (w/w), but with different aqueous phase contents. For the purposes of comparison, Al2O3 particles were also synthesised in the corresponding emulsion and by direct precipitation from aqueous solution. Nano-sized Al2O3 particles were only obtained via microemulsions, whereas the emulsion route led to hollow ball-shaped particles with sub-micron apparent sizes and the direct precipitation process resulted in angular particles about 250 nm in dimension. The nanoparticles synthesised in the microemulsion with 20 wt% aqueous phase content have smaller particle sizes (5–15 nm) and a lower transformation temperature into α-form Al2O3 crystallites. Pure α-Al2O3 nanocrystals were obtained by calcination at 1000 °C for 12 h, while the nano-sized dimension of the particles retained though the apparent particle size increased to some extent. This transformation temperature is about 200 °C lower than that for the Al2O3 particles synthesised by direct precipitation.

Effect of acetylacetone on the preparation of PZT materials in sol-gel processing

Abstract Sol–gel processing is an advantageous route to produce PZT thin film materials with high quality. PZT powders and thin films with good properties were fabricated by sol–gel processing, using acetylacetone as modifier, in the study. The morphologies of PZT powders and thin films were observed by field emission microscopy, and the dielectric and properties of the PZT thin films were measured. Thermal analysis, XRD and FTIR were used to investigate the influence of ligands on the phase transformation in PZT materials, and it is found that the difficulty of decomposing acetylacetone ligands completely resulted in a higher pyrolysis temperature to form PZT with pure phase.

Surface Characteristics of Polyhedral Oligomeric Silsesquioxane Modified Clay and Its Application in Polymerization of Macrocyclic Polyester Oligomers

Novel porous aminopropyllsooctyl polyhedral oligomeric silsesquioxane (POSS) modified montmorillonite clay complexes (POSS-Mts) with large interlayer distance and specific surface area have been successfully prepared via ion-exchange reaction and followed by freeze-drying treatment. The morphology of the POSS-Mts is highly influenced by the POSS concentration, pH of the suspension and drying procedure, but the interlayer distance of the POSS-Mts does not change much when the POSS concentration is above 0.4 CEC. The POSS-Mts were used as Sn-catalyst supporters to initiate the ring-opening polymerization of cyclic butylene terephthalate oligomers (CBT) for the first time. No diffraction peak was detected by wide-angle X-ray diffraction for the polymerized composites (pCBT/POSS-Mt), even at 10 wt % loading of POSS-Mt. A clay network rather than exfoliation structure was observed unexpectedly in the composites by transmission electron microscopy. The pCBT/POSS-Mt composite with 10 wt % POSS-Mt was further melt-compounded with commercial PBT resin as a master batch. The tensile properties of the resultant PBT/POSS-Mt composites were highly improved as compared to the pristine PBT due to the homogeneous dispersion of POSS-Mt in the PBT matrix.

The structure of ceramic foams produced using polymeric precursors

During the last decade porous ceramic materials have been finding increasing applications due to their favorable properties such as high temperature stability, high permeability, low mass, low specific heat capacity and low thermal conductivity. These characteristics are essential for many technological applications such as catalyst supports, filters for molten metals and hot gases, refractory linings, thermal and fire insulators and porous implants [1, 2]. Ceramic foams can be produced by different methods, principally impregnation of polymer foams with slurries containing appropriate binders and ceramic particles followed by pressureless sintering at elevated temperatures [2–5]. This involves coating an open-cell polymeric sponge with a ceramic slurry several times, pyrolysis of the polymer to form a ceramic skeleton followed by sintering. Ceramic foams produced by this method are generally of low strength as their struts are thin and can contain a hole in the center [2, 6–8]. Recently, a new method to produce silicon carbide (SiC) foams using polymeric precursor solutions was developed by Bao et al. [9] where a polyurethane foam was immersed in a polymeric precursor solution to form a pre-foam which was pyrolyzed in nitrogen. The main advantages of this new approach are the simplicity and ease of control of structure of the final product. This new process was exploited further to prepare silicon carbide-silicon nitride (SiC-Si3N4) composite foams [10]. In this letter we provide microstructural evidence of the improvements in structure of the ceramic foams produced by our method. The polysilane precursor discussed in this study was synthesized by the alkali dechlorination of a combination of chlorinated silane monomers in refluxing toluene/tetrahydrofuran with molten sodium as described previously [11, 12]. The structure of the SiC polysilane precursor synthesized is given below. Ph indicates a phenyl group.

Different strategies for the synthesis of silicon carbide-silicon nitride composites from preceramic polymers

Three strategies for the synthesis of silicon carbide–silicon nitride composites from organosilicon preceramic polymers were investigated. Firstly, polymeric precursors with reactive groups for silicon carbide and silicon nitride were synthesized, blended and pyrolyzed. Secondly, a polymeric precursor for silicon carbide was mixed with silicon powder which acts as a reactive filler and the resulting mixtures were pyrolyzed. Thirdly, a co-polycyclodisilazane–silane single polymeric precursor was synthesized and pyrolyzed. The precursors and the various stages of processing were studied using gel permeation chromatography, Fourier transform-infrared spectroscopy, thermo-mechanical analysis, thermogravimetry and X-ray diffraction. In each instance silicon carbide–silicon nitride composites were prepared successfully.

Silicon carbide–titanium carbide composite foams produced using a polymeric precursor

Abstract A polysilane solution used as a silicon carbide (SiC) precursor was mixed with different amounts of titanium carbide (TiC) powder and open cell polyurethane (PU) foams were dipped in these suspensions. The resulting pre-foams were pyrolyzed at 900°C in nitrogen and then heated further at various temperature between 1100 and 1600°C in the same atmosphere to produce SiC–TiC composite foams. The evolution of the composite foams has been studied using thermogravimetry and X-ray diffraction. The PU foam, pre-foams and the SiC–TiC composite foams were characterized by optical and scanning electron microscopy. These studies show that the pre-foams retained their shape well during pyrolysis and the composite foams produced consist of an open cell structure and hole-free solid struts. Prevention of cracking in the foams were dependent on the TiC content. The shrinkage observed during the conversion of the pre-foams to the composite ceramic foams can be controlled by varying the TiC content and the sintering temperature.

Smectic Phases Observed in 1, 1,2,2,-tetrahydroperfluoroalkyl-4-nitrobenzoates

On studying the thermal behaviour of a series of 1,1,2,2-tetrahydro-perfluoroalkyl 4-nitrobenzoates it was found that the decyl and dodecyl compounds showed smectic mesophases. This illustrates that a polar substituent in the 3-position of the aromatic ring for 1,1,2,2-tetrahydroperfluoroalkylbenzoates is not a requirement for thermotropic behaviour.