Fabrication of Functionally Graded Hybrid Composites TEAM MEMBERS

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Fabrication of Functionally Graded Hybrid Composites TEAM MEMBERS Texas A&M University Ibrahim Karaman (Mechanical Engineering) Zoubeida Ounaies (Aerospace Engineering) Miladin Radovic (Mechanical Engineering) University of Illinois UC Scott White (Aerospace Engineering) University of Dayton Khalid Lafdi (Mechanical and Aerospace Engineering) Research Institute Virginia Tech Dan Inman (Mechanical Engineering) Stanford University Fu Kuo Chang (Aeronautics and Astronautics)

(FGHCs) The concept Materials MAX Phase Metal layer (Ti or SMA) ~ 1000 C Oxide ceramic Functionally graded ceramic/ metal composite (GCMeC) MAX Phase Mg, Ti, Shape Memory Alloys ~ 400 C Polymer matrix composite (PMC) self-healing damaged protective oxide surface Ti2AlC (light) + γtial (dark) as 15 µm thick protective Al2O3 surface layer formed after 10,000 an example of MAX phase (Produced by Spark Functionally Hybridcomposite. Composites heating cycles of TiGraded 2AlC Plasma Sintering) Function Thermal/Environmental Barrier Coating (Al2O3, ZrO2, PS-ZrO2) Self-healing of Protective Coating Gradual Change in Thermal Expansion Thermal Management Mechanical Damping Compressive Stress on Ceramic Load Bearing Host Sensors Damage Propagation Barrier woven fibers 0.5 mm cross sec+on view 0.5 mm Actively Cooled PMC with microvascular cooling functionality and/or High Temperature PMCs with polyimide matrices

(FGHCs) The team Fabrication of Polymer Matrix Composites (PMCs) Radovic (TAMU Ceramics and MAX phases) Karaman (TAMU Ti alloys and SMAs) High Actively ActivelyCooled Cooled High Temperature Temperature PMCs PMCs PMCs White White (UIUC) (UIUC), Ounaies (TAMU) Ounaies (TAMU) Ounaies, Radovic, Karaman (TAMU) Lafdi (UDRI) Inman (VTU) Chang (Stanford)

Fabrication of MAX Phases and GCMeCs Materials: Ti 2 AlC or Ti 3 SiC 2 (MAX phases), Ti and SMAs (NiTi, NiTiPd, MnPd) Forming MAX Phases! Reaction Sintering from Elemental Powders! Hot Pressing (HP)! Hot Isostatic Pressing (HIP)! Sintering of MAX Phase Powders (Ti 3 SiC 2 and Ti 2 AlC)! HP, HIP, Tape Casting! Slip Casting! Extrusion! Establish MAX phase porous preforms Infiltration of molten metal Pressureless Suction casting Forced infiltration Excess amount of metallic powders A GCMeC layer Or co-sintering using SPS

Fabrication of GCMeCs TiAl/Ti 2 AlC composites were produced by spark plasma sintering technology from mixed powders of Ti, Al and TiC. Pressureless melt infiltration of Mg in Ti 2 AlC porous perform.! S. Amini, Composites Sci. Tech., 69 (2009) B. Mei, Journal of Materials Science 75 (2002)

Attributes of MAX Phases and GCMeCs 10µm Very good damage tolerance Large plastic deformation at high temps Excellent machinability High stiffness Ultrasound attenuation is a function of the applied load can be used for stress/health monitoring. Good combination of mechanical properties and corrosion resistance Ti based alloys or shape memory materials are expected to have excellent bonding with MAX phases, and provide high damping capacity and compressive stresses imposed at high temperatures due to shape memory effect.

Key Technical Challenges Control phase fractions and distribution including gradual change in phase distribution through the thickness; Control over phase distribution using different processing approaches: Infiltration Reactive sintering Co-sintering Interfacial integrity between metal and ceramic particles and layers Both candidate alloys and ceramics have Ti. Long term chemical compatibility between metal and ceramic phases, and between layers with different amount of phases; Full infiltration of molten metal into porous MAX phase preform.

PMC Layer Actively-Cooled PMCs (AC-PMCs): Microvascular Composites MAX Phase Mg, Ti, Shape Memory Alloys AC-PMC Concepts Short term: 2D planar array of embedded microchannels layered within a PMC 3-D Woven Microvascular Composites. 3D orthogonally woven monolith with 56% fiber content Long term: 3D woven PMC architectures with integrated microvascular networks with sacrificial fibers co-mingled with reinforcement tows

2D Planar Arrays Leveraging of preliminary work accomplished under AFOSR MURI on Microvascular Autonomic Composites at UIUC 5 mm! 3 x 24 x 200 µm channel grid network!

Preliminary Results

3D Woven PMC Microvascular networks embedded in 3D woven PMC that provide active cooling capability Sacrificial fibers integrated in z-tows (and/or x- and y-) that are removed during post-cure operation permanent tow sacrificial tow Schematic of sacrificial fibers integrated with the 3D preform weave

Key Technical Challenges Sacrificial fiber development Adequate hardness, extensibility, bend strength, etc. Tailorable phase transition for post-cure removal Thermal melt, thermal depolymerization and volatilization, solvent extraction Optimization of vascular network architectures Easy post-cure removal + high thermal efficiency/low flow resistance Weaving and co-mingling of sacrificial and structural fibers Collaboration: 3Tex, TEAM Fabrication of Composites RTM/VARTM Flow characterization and defect analysis (µ-ct, etc.)

Approach PMC Layer High-Temperature PMCs (HT-PMCs): Polyimide-Based Composites Several polyimide matrices with T g up to 400 o C including bismaleimidebased polyimides (Maverick Co. and AFRL) Available in powder or solution form Processing Depending on viscosity: Solution-cast, Thermal Cure then Autoclave Advantages Solvent-assisted Resin Transfer Molding Polyimides have good thermo-oxidative stability, resistance to moisture absorption, and relatively high moduli. Polyimides can withstand hot spikes up to two times their T g.

Key Technical Challenges High-Temperature PMCs (HT-PMCs): Polyimide-Based Composites Viscosity of aromatic HT polyimides tends to be elevated which makes processing a challenge Solvent-assisted processing of polymer to control viscosity. Composite processing by infusing fibers and fabric RTM/VARTM or autoclave for composite processing. Effect on T g and thermal/structural properties. Coupon fabrication using fuzzy glass or fuzzy SiC fibers for SHM

Joining GCMeC and PMC The GCMeC/PMC interface consists of bonding the pure metal to the polymer matrix. Three joining approaches are adopted: bonding of metal to PMC using vertical nanocolumns followed by resin infusion, bonding of metal to an intermediate fabric preform using vertical columns grown on both surfaces, with subsequent infusion of resin, using Z-pinning technology

Joining GCMeC and PMC Z-Pin Locking Metal infiltration in the porous ceramic using a hot press or SPS. Pressing die with small, high aspect ratio holes to create metallic micropillars as Z- pins. Alternately, micromachining to create Z- pins. Mechanical locking as the polymer resin is flown on top of the metal layer then cured.

Joining GCMeC and PMC Vertical Nanocolumns Vertical nanocolumns are grown forest of carbon nanotubes using CVD. Carbon nanotubes grown on Niwire 1) Forest will be grown directly on metal layer Polymer will be infused to fill voids between nanotubes Pressing to the rest of composite preform then curing. 2) Forest will be grown on metal layer and fiber fabric Polymer will be infused to fill voids between nanotubes Pressing then curing.

SUMMARY Collaboration is the key to success Phase distribution, interface chemistry and properties, thermal and structural properties, etc. 1000 C 300-400 C Fabrication Multi-scale Characterization Joining PMC w/ GCMeC, embedded SHM sensors Structural Health Monitoring Initial material parameters Validation experiments Phase distribution and morphology, layer thickness, reinforcement and cooling network distribution, and desired functional grading for thermal management and structural properties Multiscale Structural Modelling