Development and Characterization of Continuous SiC Fiber‐Reinforced HfB2‐Based UHTC Matrix Composites Using Polymer Impregnation and Slurry Infiltration Techniques

This paper discusses the development of continuous SiC fiber‐reinforced HfB₂‐SiC composite laminates. A range of techniques, based on resin‐based precursors and slurries, for infiltrating porous SiC preforms with HfB₂ powder were developed. While resin‐based precursors proved to be ineffective due to low HfB₂ yield and poor adhesion, the slurry infiltration techniques were effective to varying degrees. The greatest pore filling and composite densities were achieved using pressure and vibration‐assisted pressure infiltration techniques. SiC_f/HfB₂‐SiC laminates were subsequently developed via lamination, cure and pyrolysis of fabrics using a HfB₂‐loaded polymeric SiC precursor, followed by HfB₂ slurry infiltration and preceramic polymer infiltration and pyrolysis (PIP). Repeated PIP processing, for 6–10 cycles, resulted in density increases, from the 3.03–3.22 g/cm³ range after HfB₂ slurry infiltration, to 3.97–4.03 g/cm³ after PIP processing. Correspondingly, there was a decrease in open porosity from approximately 52% to less than 11%. The matrix consisted of discreet, lightly sintered HfB₂ particles dispersed in SiC. The PIP SiC matrix was primarily nanocrystalline after 1300°C pyrolysis, but experienced grain growth with further heat treatment at 1600°C.     

Monazite Coatings on Fibers: I, Effect of Temperature and Alumina Doping on Coated-Fiber Tensile Strength

Monazite was continuously coated onto Nextel 720 fibers, using an aqueous precursor and in-line heat treatment at 900°–1300°C. Some experiments were repeated with alumina-doped precursors. Coated fibers were heat-treated for 100 h at 1200°C. Coatings were characterized by optical microscopy, scanning electron microscopy, and analytical transmission electron microscopy. Coated-fiber tensile strengths were measured by single-filament tensile tests. The precursors were characterized by X-ray diffractometry, differential thermal analysis/thermogravimetric analysis, and mass spectrometry. Coated-fiber tensile strength was lower for fibers coated at higher deposition temperatures. Heat treatment for 100 h at 1200°C decreased tensile strength further. The coatings were slightly phosphate-rich and enhanced alumina grain growth at the fiber surface, but phosphorus was not detected along the alumina grain boundaries. Fibers with alumina-doped coatings had higher tensile strengths than those with undoped coatings after heat treatment for 100 h at 1200°C. Alumina added as α-alumina particles gave higher strengths than alumina added as colloidal boehmite. Alumina doping slowed monazite grain growth and formed rough fiber–coating interfaces after 100 h of heat treatment at 1200°C. Possible relationships among precursor characteristics, coating and fiber microstructure development, and strength-degradation mechanisms are discussed in this paper.     

Monazite Coatings on SiC Fibers I: Fiber Strength and Thermal Stability

Commercially available SiC fibers were coated with monazite (LaPO₄) using a continuous vertical coater at 1100°C. Coated fibers were heat treated in dry air, argon, and laboratory air at 1200°C for 1–20 h. The tensile strengths of uncoated and coated fibers were measured and evaluated before and after heat treatment. Fiber coating did not degrade SiC fiber strength, but heat treatment afterwards caused significant degradation that correlated with silica scale thickness. Possible strength degradation mechanisms for the coated fibers are discussed. Coating morphology, microstructure, and SiC oxidation were observed with scanning electron microscopy and transmission electron microscopy. Monazite reacted with SiC to form lanthanum silicate (La₂Si₂O₇) in argon, but was stable with SiC in air. Despite the large coefficient of thermal expansion difference between monazite and SiC, micron thick monazite coatings did not debond from most types of SiC fibers. Possible explanations for the thermomechanical stability of the monazite fiber coatings are discussed.     

Fabrication and Testing of Oxide/Oxide Microcomposites with Monazite and Hibonite as Interlayers

Oxide/oxide microcomposites were fabricated and tested to evaluate the effectiveness of monazite (LaPO₄) and hibonite (CaAl₁₂O₁₉) as interlayers in sapphire-reinforced Al₂O₃-matrix composites. For interlayer thicknesses of 0.3-0.5 µm, both interlayers showed evidence of crack deflection; however, debond lengths in hibonite-coated specimens were limited to just a small fraction of the fiber diameter. Monazite-coated specimens showed multiple matrix cracks and extensive debonding at the coating/matrix interface. Composite strengths were relatively high for both coatings, considering the fiber strength degradation during processing. The strengths were greater than the calculated matrix cracking stresses. However, the mean strengths were not significantly different from those of the control specimens, although coated composites had higher Weibull moduli. The lack of difference in strength is attributed to porosity in the matrix. The results imply that matrix density needs to be >85% to evaluate novel interface strategies reliably.     

Precipitation Coating of Rare-Earth Orthophosphates on Woven Ceramic Fibers—Effect of Rare-Earth Cation on Coating Morphology and Coated Fiber Strength

Monazite (La, Ce, Nd, and GdPO₄) and xenotime (Tb, Dy, and YPO₄) coatings were deposited on woven Nextel^™ 610 and 720 fibers by heterogeneous precipitation from a rare-earth citrate/phosphoric acid precursor. Coating phases and microstructure were characterized by SEM and TEM, and coated fiber strength was measured after heat treatment at 1200°C for 2 h. Coated fiber strength increased with decreasing ionic radius of the rare-earth cation in the monazite and xenotime coatings, and correlates with the high-temperature weight loss and the densification rate of the coatings. Dense coatings with trapped porosity and high weight loss at a high temperature degrade fiber strength the most. The degradation is consistent with stress corrosion driven by thermal residual stress from coating precursor decomposition products trapped in the coating at a high temperature.     

Modification of absorbent poly(glycerol‐glutaric acid) films by the addition of monoglycerides

Monoglycerides (MGs) have been incorporated into the matrix of poly(glycerol‐co‐glutaric acid) films to investigate their effect on the thermal, mechanical, and solvent absorption properties of the resultant films. Solvent absorption studies revealed that poly(glycerol‐co‐glutaric acid‐co‐MG) films were able to absorb and resorb solvents better than poly(glycerol‐co‐glutaric acid) films, albeit they had higher erosion levels. Thermogravimetric analysis showed that the incorporated MGs did not affect the thermal stability of the glycerol‐based films. The MG‐incorporated films were observed to be much softer than the poly(glycerol‐co‐glycerol) films which was further proven by a 39‐fold reduction in Young's Modulus and 17‐fold reduction in fracture energy when compared to the poly(glycerol‐co‐glycerol). Mechanical property studies also revealed that the incorporation of MGs increased the elongation % and reduced the tensile strength of poly(glycerol‐co‐glutaric acid) films. Correlation analysis revealed a strong linear relationship between Young's Modulus and fracture energy (R² = 0.9962), and between Young's Modulus and tensile strength (R² = 0.9972). Our study proved that MGs can be successfully incorporated in the polymer matrix of poly(glycerol‐co‐glutaric acid) films to produce softer films with increased elongation and increased solvent absorption capacity. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45381.     

Comprehensive numerical modelling of the hot isostatic pressing of Ti-6Al-4V powder: From filling to consolidation

Hot Isostatic Pressing (HIP) is a manufacturing process for production of near-net-shape components, where models based on Finite Element Method (FEM) are generally used for reducing the expensive experimental trials for canister design. Researches up to date implement in the simulation a uniform powder relative density distribution prior HIPping. However, it has been experimentally observed that the powder distribution is inhomogeneous after filling, leading to a non-uniform tool shrinkage. In this study a comprehensive numerical model for HIPping of Ti-6Al-4V powder is developed to improve model prediction by simulating powder filling and pre-consolidation by means of a two-dimensional Discrete Element Method (DEM). Particles’ dimension has been scaled up in order to reduce the computational cost of the analysis. An analytical model has been developed to calculate the relative density distribution from powder particle distribution provided by DEM, which is then passed in information to a three-dimensional FEM implementing the Abouaf and co-workers model for simulating powder densification during HIPping. Results obtained implementing the initial relative density distribution calculated from DEM are compared with those obtained considering a uniform relative density distribution over the powder domain (classic approach) at the beginning of the analysis. Experimental work has been carried out for validating the DEM (filling) and FEM (HIP) model. Comparison between experimental and numerical results shows the ability of the DEM model to represent the powder flow during filling and pre-consolidation, providing also a reliable values of the relative density distribution. It also highlights that taking into account the non-uniform powder distribution inside the canister prior HIP is vital to improve numerical results and produce near-net-shape components.     

Synthesis of absorbent polymer films made from fatty acid methyl esters,glycerol, and glutaric acid: Thermal,mechanical, and porosity analyses

In previous studies, monoglycerides (MGs) were incorporated into the matrix of poly(glutaric acid–glycerol) films to investigate their effect on the thermal, mechanical, and solvent absorption properties of the resultant films. In this study, the same properties were monitored when fatty acid methyl esters (FAME) were added to the polymer film formulation. Thermogravimetric analysis showed that, while the decomposition profile of the FAME and MG-infused films were different, the final decomposition temperatures were similar for both film types at approximately 400 °C. Degree of branching (DB%) was calculated from nuclear magnetic resonance data and was used to examine the effect of DB% on the mechanical and absorption properties of the films. Experimental results did not show any correlation with DB% and any of the physical, chemical, mechanical, or thermal properties studied. Relative to the poly(glycerol–glutaric acid) control, the incorporation of MG into the polymer matrix resulted in improved % absorption but decreased the mechanical property values. Conversely, adding FAME into the matrix improved the mechanical property values; however, there was no significant change in the % absorption values relative to the control. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47822.