The rheological properties of commercially available polycarbosilane, SMP-10, were analyzed as a function of temperature, to guide development of thermal treatment processes for the improved yield and functionality of polymer ceramic precursors. The curing onset temperature for SMP-10 was determined to be as low as 100°C for a heating rate of 1°C/min enabling a heat treatment process at 90°C, where low molecular weight oligomers volatilize from the liquid precursor prior to curing. By driving off the low molecular weight oligomers before fabrication of a composite, the mass yield of SMP-10, from a room temperature liquid state was increased from 77% to 83%. The development of B-staging processes, or a semicure of SMP-10, were also demonstrated. B-staging processes were then applied to polymer infiltration and pyrolysis processing and compared with traditional wet layup CMC processing. It was determined that B-staging processes did not adversely affect ceramic matrix composite fabrication. B-staged processing methods were determined to result in less waste, allow ply-by-ply control of matrix compositions, and enable time independent processing when compared to traditional wet layup processing methods. K E Y W O R D Sceramic matrix composites, microstructure, pre-ceramic polymers, silicon carbide
The volatilization of polycarbosilanes is important to the processing and performance of polymer infiltration and pyrolysis‐based ceramic matrix composites. Low molecular weight (MW) polycarbosilane is often present in preceramic polymers and enhances viscosity for the purpose of composite infiltration. Due to the volatility of low MW chains, a model was developed to semi‐empirically determine the MW distribution and then predict the mass yield and evolution of the MW distribution as a function of temperature and time for StarPCS™ SMP‐10. The enthalpy of vaporization, the temperature dependence of the enthalpy of vaporization, the temperature dependence of the normal boiling point and a representation of the molecular weight distribution were fit using a series of thermogravimetric measurements, involving isothermal holds on a particular batch of SMP‐10. Once calibrated for SMP‐10 in this fashion, the molecular weight distribution of different batches of SMP‐10 could be fit using a thermogravimetric measurement involving a reduced temperature‐time series. The model was then predictive of mass loss over time for temperatures below the onset of curing (>90°C). Understanding this volatilization enables improved SiC yield, reduced processing time and minimizing void/bubble formation.
Ceramics consisting of titanium diboride with titanium carbide additions were fusion welded to produce continuous joins. A welding current of 135 A, welding speed of 8 cm/min, and plasma flow rate of 0.75 L/min were combined with a preheat temperature of ~1450°C to fusion weld coupons of TiB2 containing 20 vol% TiC with a thickness of 4 mm. The resulting fusion zone (FZ) was 3.9 mm deep at the center of the joint and 10.4 mm wide. During cooling of the melt pool, four distinct regions of crystal growth and nucleation were observed due to thermal gradients. Regions at the top and bottom of the FZ exhibited smaller TiB2 crystals due to higher nucleation rates whereas regions in the middle of the FZ showed higher growth rates, with TiB2 crystals up to 1.2 mm in length. Thermal gradients also affected cooling of the eutectic phase, causing a cellular structure to appear in the cooled eutectic. Plasma arc welding was a viable method for joining diboride‐based ceramics.
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