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Lin, Yi

Publications and source records attributed to Lin, Yi.

At least 19 records

Reliable Bonding of Composite Laminates Using Reflowable Epoxy Resins

Epoxy matrix composites assembled with adhesives maximize the performance of aerospace structures, but the possibility of forming weak bonds requires the installation of redundant fasteners, which add weight and manufacturing cost. Co-cured joints (e.g. unitized composite structures) are immune to weak bonds because the uncured resin undergoes diffusion and mixing through the joint. A means of co-curing complex structures may reduce the need for redundant fasteners in bondlines. To this end, NASA started the AERoBOND project to develop novel joining materials to enable a “secondary-co-cure” assembly process. Aerospace epoxy resin systems reformulated with offset stoichiometry prevented the resin from advancing beyond the gel point during a conventional autoclave cure cycle up to 180 °C. The offset resins were applied to the joining surfaces of laminate preforms as prepreg. Two surfaces with complimentary offset resins were joined using conventional secondary bonding techniques. Preliminary efforts have indicated that the resulting joint has no discernable interface and appears as a conventional co-cured laminate under optical magnification. This report will discuss the initial work performed regarding formulation of the epoxy resin system using calorimetry, rheology, and mechanical testing.

Palmieri, Frank L.↗

Reinforcing Additives for Ice Adhesion Reduction Coatings

Adhesion of contaminants has been identified as a ubiquitous issue for aeronautic exterior surfaces. In-flight icing is particularly hazardous for all aircraft and can be experienced throughout the year under the appropriate environmental conditions. On larger vehicles, the accretion of ice could result in loss of lift, engine failure, and potentially loss of vehicle and life were it not for active deicing or anti-icing equipment. Smaller vehicles though cannot support the mass and mechanical complexity of active ice mitigating systems and thus must rely upon passive approaches or avoid icing conditions altogether. One approach that may be applicable to all aircraft is the use of coatings. Durability remains an issue and has prevented realization of coatings for leading edge contamination mitigation. In this work, epoxy coatings were generated as a passive approach for ice adhesion mitigation and methods to improve durability were evaluated. Highly cross-linked epoxy systems can be extremely rigid, which could have deleterious consequences regarding application as a leading edge coating. Incorporation of flexible species, such as poly(ethylene glycol) may improve coating toughness.8 Additionally, core-shell rubber (CSR) particles have been utilized to improve fracture toughness of epoxies.9 Both of these more established additives are investigated in this work. An emerging additive that is also evaluated here is holey graphene. This nanomaterial possesses many of the advantageous properties of graphene (excellent mechanical properties, thermal and electrical conductivity, large surface area, etc.) while also exhibiting behaviors associated with flexible, porous materials (i.e., compressibility, increased permeation, etc.). Holey graphene, HG, was synthesized by the oxidation of defect-rich sites on graphene sheets through controlled thermal expo-sure.10 It is envisioned that the porous nature of HG would allow resin penetration through the graphitic plane, resulting in better interfacial interaction and therefore better translation of the nanomaterial’s properties to the surrounding matrix.

Wohl, Christopher J↗

Optimization of Picosecond Laser Parameters for Surface Treatment of Composites Using a Design of Experiments (DOE) Approach

Based on guidelines from the Federal Aviation Administration, research supported by the NASA Advanced Composites Project is investigating methods to improve process control for surface preparation and pre-bond surface characterization on aerospace composite structures. The overall goal is to identify high fidelity, rapid, and reproducible surface treatments and surface characterization methods to reduce the uncertainty associated with the bonding process. The desired outcome is a more reliable bonded airframe structure, and to reduce time to achieve certification. In this work, a design of experiments (DoE) approach was conducted to determine optimum laser ablation conditions using a pulsed laser source with a nominal pulse width of 10 picoseconds. The laser power, frequency, scan speed, and number of passes (1 or 2) were varied within the laser system operating boundaries. Aerospace structural carbon fiber reinforced composites (Torayca® 3900-2/T800H) were laser treated, then characterized for contamination, and finally bonded for mechanical testing. Pre-bond characterization included water contact angle (WCA) using a handheld device, ablation depth measurement using scanning electron microscopy (SEM), and silicone contamination measurement using laser induced breakdown spectroscopy (LIBS). In order to accommodate the large number of specimens in the DoE, a rapid-screening, double cantilever beam (DCB) test specimen configuration was devised based on modifications to ASTM D5528. Specimens were tested to assess the failure modes observed under the various laser surface treatment parameters. The models obtained from this DoE indicated that results were most sensitive to variation in the average laser power. Excellent bond performance was observed with nearly 100% cohesive failure for a wide range of laser parameters. Below about 200 mW, adhesive failure was observed because contamination was left on the surface. For laser powers greater than about 600 mW, large amounts of fiber were exposed, and the failure mode was predominately fiber tear.

Palmieri, Frank L.↗

Determination of Trace Silicone Contamination on Composites by Quantitative XPS and LIBS

Surface treatment and surface characterization techniques are critical to ensure that adherends are chemically activated and free of contaminants prior to adhesive bonding. Silicone contamination from mold-release agents and other sources can interfere with interfacial bonding, decreasing the durability and performance of bonded composite structures. Tools and methods are needed that can be used in a production environment to reliably detect low levels of contaminants in a rapid, simple, and cost-effective manner to improve bond reliability. In this work, surface characterization of carbon fiber reinforced polymer (CFRP) composites was performed using laser induced breakdown spectroscopy (LIBS) and the results were compared with those obtained from X-ray photoelectron spectroscopy (XPS). The objective was to investigate the ability to quantify the surface species measured by LIBS since it offers many advantages over XPS in terms of ease of use, sample preparation, and real-time results. The as-processed CFRP panels had trace surface silicone contamination from the fabrication process, the source of which was not investigated. The composites were laser treated at select average laser power levels, resulting in varying levels of contamination reduction. The Si atomic percentage measurements using XPS were conducted both before and after laser ablation. The XPS results were compared with those obtained from LIBS to assess the reliability of each technique for surface contaminant characterization. The results showed an excellent correlation in Si atomic concentration between the two techniques.

Ledesma, Rodolfo↗

Picosecond Pulsed Laser Ablation for the Surface Preparation of Epoxy Composites

As part of a technical challenge under the Advanced Composites Program, methods for improving pre-bond process control for aerospace composite surface treatments and inspections, in conjunction with Federal Aviation Administration guidelines, are under investigation. The overall goal is to demonstrate high fidelity, rapid and reproducible surface treatment and surface characterization methods to reduce uncertainty associated with the bonding process. The desired outcomes are reliable bonded airframe structure, and reduced timeline to certification. In this work, laser ablation was conducted using a q-switched Nd:YVO4 laser capable of nominal pulse durations of 8 picoseconds (ps). Aerospace structural carbon fiber reinforced composites with an epoxy resin matrix were laser treated, characterized, processed into bonded assemblies and mechanically tested. The characterization of ablated surfaces were conducted using scanning electron microscopy (SEM), water contact angle (WCA) goniometry, micro laser induced breakdown spectroscopy (uLIBS), and electron spin resonance (ESR). The bond performance was assessed using a double cantilever beam (DCB) test with an epoxy adhesive. The surface characteristics and bond performance obtained from picosecond ablated carbon fiber reinforced plastics (CFRPs) are presented herein.

Palmieri, Frank↗

Single-Step, Solvent-Free, Catalyst-Free Preparation of Holey Carbon Allotropes

Methods for forming holey carbon allotropes and graphene nanomeshes are provided by the various embodiments. The various embodiments may be applicable to a variety of carbon allotropes, such as graphene, graphene oxide, reduced graphene oxide, thermal exfoliated graphene, graphene nanoribbons, graphite, exfoliated graphite, expanded graphite, carbon nanotubes (e.g., single-walled carbon nanotubes, double-walled carbon nanotubes, few-walled carbon nanotubes, multi-walled carbon nanotubes, etc.), carbon nanofibers, carbon fibers, carbon black, amorphous carbon, fullerenes, etc. The methods may produce holey carbon allotropes without the use of solvents, catalysts, flammable gas, additional chemical agents, or electrolysis to produce the pores (e.g., holes, etc.) in the carbon allotropes. In an embodiment, a carbon allotrope may be heated at a working window temperature for a working period of time to create holes in the carbon allotrope.

Lin, Yi↗

Controlled Contamination of Epoxy Composites with PDMS and Removal by Laser Ablation

Surface preparation is critical to the performance of adhesively bonded composites. During manufacturing, minute quantities of mold release compounds are inevitably deposited on faying surfaces and may compromise bond performance. To ensure safety, mechanical fasteners and other crack arrest features must be installed in the bondlines of primary structures, which negates some advantages of adhesively bonded construction. Laser ablation is an automated, repeatable, and scalable process with high potential for the surface preparation of metals and composites in critical applications such as primary airframe structures. In this study, laser ablation is evaluated on composite surfaces for the removal of polydimethylsiloxane (PDMS), a common mold release material. Composite panels were contaminated uniformly with PDMS film thicknesses as low as 6.0 nm as measured by variable angle spectroscopic ellipsometry. Bond performance was assessed by mechanical testing using a 250 F cure, epoxy adhesive and compared with pre-bond surface inspection results. Water contact angle, optically stimulated electron emission, and laser induced breakdown spectroscopy were used to characterize contaminated and laser ablated surfaces. The failure mode obtained from double cantilever beam tests correlated well with surface characterization data. The test results indicated that even low levels of PDMS were not completely removed by laser ablation.

Palmieri, Frank↗

Amorphous Carbon-Boron Nitride Nanotube Hybrids

A method for joining or repairing boron nitride nanotubes (BNNTs). In joining BNNTs, the nanotube structure is modified with amorphous carbon deposited by controlled electron beam irradiation to form well bonded hybrid a-C/BNNT structures. In repairing BNNTs, the damaged site of the nanotube structure is modified with amorphous carbon deposited by controlled electron beam irradiation to form well bonded hybrid a-C/BNNT structures at the damage site.

Kim, Jae Woo↗

Flexible Micropost Arrays for Shear Stress Measurement

Increased fuel costs, heightened environmental protection requirements, and noise abatement continue to place drag reduction at the forefront of aerospace research priorities. Unfortunately, shortfalls still exist in the fundamental understanding of boundary-layer airflow over aerodynamic surfaces, especially regarding drag arising from skin friction. For example, there is insufficient availability of instrumentation to adequately characterize complex flows with strong pressure gradients, heat transfer, wall mass flux, three-dimensionality, separation, shock waves, and transient phenomena. One example is the acoustic liner efficacy on aircraft engine nacelle walls. Active measurement of shear stress in boundary layer airflow would enable a better understanding of how aircraft structure and flight dynamics affect skin friction. Current shear stress measurement techniques suffer from reliability, complexity, and airflow disruption, thereby compromising resultant shear stress data. The state-of-the-art for shear stress sensing uses indirect or direct measurement techniques. Indirect measurements (e.g., hot-wire, heat flux gages, oil interferometry, laser Doppler anemometry, small scale pressure drag surfaces, i.e., fences) require intricate knowledge of the studied flow, restrictive instrument arrangements, large surface areas, flow disruption, or seeding material; with smaller, higher bandwidth probes under development. Direct measurements involve strain displacement of a sensor element and require no prior knowledge of the flow. Unfortunately, conventional "floating" recessed components for direct measurements are mm to cm in size. Whispering gallery mode devices and Fiber Bragg Gratings are examples of recent additions to this type of sensor with much smaller (m) sensor components. Direct detection techniques are often single point measurements and difficult to calibrate and implement in wind tunnel experiments. In addition, the wiring, packaging, and installation of delicate micro-electromechanical devices impede the use of most direct shear sensors. Similarly, the cavity required for sensing element displacement is sensitive to particulate obstruction. This work was focused on developing a shear stress sensor for use in subsonic wind tunnel test facilities applicable to an array of test configurations. The non-displacement shear sensors described here have minimal packaging requirements resulting in minimal or no disturbance of boundary layer flow. Compared to previous concepts, device installation could be simple with reduced cost and down-time. The novelty lies in the creation of low profile (nanoscale to 100 μm) micropost arrays that stay within the viscous sub-layer of the airflow. Aerodynamic forces, which are related to the surface shear stress, cause post deflection and optical property changes. Ultimately, a reliable, accurate shear stress sensor that does not disrupt the airflow has the potential to provide high value data for flow physics researchers, aerodynamicists, and aircraft manufacturers leading to greater flight efficiency arising from more in-depth knowledge on how aircraft design impacts near surface properties.

Wohl, Christopher J.↗

Toward Edge-Defined Holey Boron Nitride Nanosheets

"Holey" two-dimensional (2D) nanosheets with well-defined holy morphology and edge chemistry are highly desirable for applications such as energy storage, catalysis, sensing, transistors, and molecular transport/separation. For example, holey grapheme is currently under extensive investigation for energy storage applications because of the improvement in ion transport due to through the thickness pathways provided by the holes. Without the holes, the 2D materials have significant limitations for such applications in which efficient ion transport is important. As part of an effort to apply this approach to other 2D nanomaterials, a method to etch geometrically defined pits or holes on the basal plane surface of hexagonal boron nitride (h-BN) nanosheets has been developed. The etching, conducted via heating in ambient air using metal nanoparticles as catalysts, was facile, controllable, and scalable. Starting h-BN layered crystals were etched and subsequently exfoliated into boron nitride nanosheets (BNNSs). The as-etched and exfoliated h-BN nanosheets possessed defined pit and hole shapes that were comprised of regulated nanostructures at the edges. The current finding are the first step toward the bulk preparation of holey BNNSs with defined holes and edges.

Lin, Yi↗

Bulk Preparation of Holey Graphene via Controlled Catalytic Oxidation

A scalable method allows preparation of bulk quantities of holey carbon allotropes with holes ranging from a few to over 100 nm in diameter. Carbon oxidation catalyst nanoparticles are first deposited onto a carbon allotrope surface in a facile, controllable, and solvent-free process. The catalyst-loaded carbons are then subjected to thermal treatment in air. The carbons in contact with the carbon oxidation catalyst nanoparticles are selectively oxidized into gaseous byproducts such as CO or CO.sub.2, leaving the surface with holes. The catalyst is then removed via refluxing in diluted nitric acid to obtain the final holey carbon allotropes. The average size of the holes correlates strongly with the size of the catalyst nanoparticles and is controlled by adjusting the catalyst precursor concentration. The temperature and time of the air oxidation step, and the catalyst removal treatment conditions, strongly affect the morphology of the holes.

Watson, Kent↗

Shear Stress Sensing with Elastic Microfence Structures

In this work, elastic microfences were generated for the purpose of measuring shear forces acting on a wind tunnel model. The microfences were fabricated in a two part process involving laser ablation patterning to generate a template in a polymer film followed by soft lithography with a two-part silicone. Incorporation of a fluorescent dye was demonstrated as a method to enhance contrast between the sensing elements and the substrate. Sensing elements consisted of multiple microfences prepared at different orientations to enable determination of both shear force and directionality. Microfence arrays were integrated into an optical microscope with sub-micrometer resolution. Initial experiments were conducted on a flat plate wind tunnel model. Both image stabilization algorithms and digital image correlation were utilized to determine the amount of fence deflection as a result of airflow. Initial free jet experiments indicated that the microfences could be readily displaced and this displacement was recorded through the microscope.

Cisotto, Alexxandra↗

Laser Surface Preparation of Epoxy Composites for Secondary Bonding: Optimization of Ablation Depth

Surface preparation has been identified as one of the most critical aspects of attaining predictable and reliable adhesive bonds. Energetic processes such as laser ablation or plasma treatment are amenable to automation and are easily monitored and adjusted for controlled surface preparation. A laser ablation process was developed to accurately remove a targeted depth of resin, approximately 0.1 to 20 micrometers, from a carbon fiber reinforced epoxy composite surface while simultaneously changing surface chemistry and creating micro-roughness. This work demonstrates the application of this process to prepare composite surfaces for bonding without exposing or damaging fibers on the surface. Composite panels were prepared in an autoclave and had a resin layer approximately 10 micrometers thick above the fiber reinforcement. These composite panels were laser surface treated using several conditions, fabricated into bonded panels and hygrothermally aged. Bond performance of aged, experimental specimens was compared with grit blast surface treated specimens using a modified double cantilever beam test that enabled accelerated saturation of the specimen with water. Comparison of bonded specimens will be used to determine how ablation depth may affect average fracture energies and failure modes.

Palmieri, Frank L.↗

Synthesis and Modification of Holey Graphene for Energy Storage

Porous graphene materials have recently drawn significant interest for energy storage applications due to the effective use of the graphitic surface area provided by the pores. Holey graphene is a type of porous graphene with pores in the form of physical through thickness holes. This type of porous graphene provides a unique morphology that allows for effective transport of molecular species through the graphene plane. Therefore, as we recently demonstrated, holey graphene could be advantageous in the preparation of electrodes in supercapacitors with high volumetric performance.1 We have developed methodologies to scalably prepare holey graphene materials with or without the use of catalysts (Figure 1).1,2 In this presentation, we will discuss the choice of synthetic strategies and experimental conditions on the morphology and physical properties of holey graphene (Figure 2) and the effect on their electrochemical properties. We will also present the results on the further modification of holey graphene to study their physical and chemical properties, especially with regard to the stability and chemical reactivity of carbons located around the edges of the holes.

Lin, Yi↗

Chemical Sharpening, Shortening, and Unzipping of Boron Nitride Nanotubes

Boron nitride nanotubes (BNNTs), the one-dimensional member of the boron nitride nanostructure family, are generally accepted to be highly inert to oxidative treatments and can only be covalently modifi ed by highly reactive species. Conversely, it is discovered that the BNNTs can be chemically dispersed and their morphology modifi ed by a relatively mild method: simply sonicating the nanotubes in aqueous ammonia solution. The dispersed nanotubes are significantly corroded, with end-caps removed, tips sharpened, and walls thinned. The sonication treatment in aqueous ammonia solution also removes amorphous BN impurities and shortened BNNTs, resembling various oxidative treatments of carbon nanotubes. Importantly, the majority of BNNTs are at least partially longitudinally cut, or "unzipped". Entangled and freestanding BN nanoribbons (BNNRs), resulting from the unzipping, are found to be approximately 5-20 nm in width and up to a few hundred nanometers in length. This is the fi rst chemical method to obtain BNNRs from BNNT unzipping. This method is not derived from known carbon nanotube unzipping strategies, but is unique to BNNTs because the use of aqueous ammonia solutions specifi cally targets the B-N bond network. This study may pave the way for convenient processing of BNNTs, previously thought to be highly inert, toward controlling their dispersion, purity, lengths, and electronic properties.

Liao, Yunlong↗