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At least 91 records · Page 5

Exploratory Study on the Effects of Novel Diamine Curing Agents and Isocyanate Precursors on the Properties of New Epoxy and Urethane Adhesives

This report covers the results of investigations directed toward studying the effects of novel aromatic diamine structures on epoxy adhesive properties and includes work done under a modification to the original contract. Three aromatic diamines based on diphenylsulfone and benzophenone were studied as epoxy adhesive curing agents. Previously found differences in adhesive strengths for meta vs para orientation were not found in these series. The use of aluminum and alumina as fillers in a m,m'-methylene dianiline-cured epoxy adhesive was not found to be beneficial to adhesive strength. Alumina filled adhesives had much lower strength than unfilled adhesives. The unfilled m,m'-methylene dianiline-based epoxy adhesive had excellent resistance to moisture relative to a p,p'-methylene dianiline-based adhesive and maintained good strengths up to 250 F. A glass fiber composite based on a m,m'-methylene dianiline-cured epoxy appeared to be equivalent to the p,p'-methylene dianiline-cured epoxy as judged by short beam shear tests.

Glasgow, D. Gerald↗

Room-Temperature-Cured Copolymers for Lithium Battery Gel Electrolytes

Polyimide-PEO copolymers (PEO signifies polyethylene oxide) that have branched rod-coil molecular structures and that can be cured into film form at room temperature have been invented for use as gel electrolytes for lithium-ion electric-power cells. These copolymers offer an alternative to previously patented branched rod-coil polyimides that have been considered for use as polymer electrolytes and that must be cured at a temperature of 200 C. In order to obtain sufficient conductivity for lithium ions in practical applications at and below room temperature, it is necessary to imbibe such a polymer with a suitable carbonate solvent or ionic liquid, but the high-temperature cure makes it impossible to incorporate and retain such a liquid within the polymer molecular framework. By eliminating the high-temperature cure, the present invention makes it possible to incorporate the required liquid.

Meador, Mary Ann B.↗

Cure Cycle Design Methodology for Fabricating Reactive Resin Matrix Fiber Reinforced Composites: A Protocol for Producing Void-free Quality Laminates

For the fabrication of resin matrix fiber reinforced composite laminates, a workable cure cycle (i.e., temperature and pressure profiles as a function of processing time) is needed and is critical for achieving void-free laminate consolidation. Design of such a cure cycle is not trivial, especially when dealing with reactive matrix resins. An empirical "trial and error" approach has been used as common practice in the composite industry. Such an approach is not only costly, but also ineffective at establishing the optimal processing conditions for a specific resin/fiber composite system. In this report, a rational "processing science" based approach is established, and a universal cure cycle design protocol is proposed. Following this protocol, a workable and optimal cure cycle can be readily and rationally designed for most reactive resin systems in a cost effective way. This design protocol has been validated through experimental studies of several reactive polyimide composites for a wide spectrum of usage that has been documented in the previous publications.

Hou, Tan-Hung↗

Relationship of Cure Temperature to Mechanical, Physical, and Dielectric Performance of PDMS Glass Composite for Electric Motor Insulation

Achieving NASAs aggressive fuel burn and emission reduction for N-plus-3 aircraft will require hybrid electric propulsion system in which electric motors driven by either power generated from turbine or energy storage system will power the fan for propulsion. Motors designed for hybrid electric aircraft are expected to operate at medium to high voltages over long durations in a high altitude service environment. Such conditions have driven research toward the development of wire insulation with improved mechanical strength, thermal stability and increased breakdown voltage. The silicone class of materials has been considered for electric wire insulation due to its inherent thermal stability, dielectric strength and mechanical integrity. This paper evaluates the dependence of these properties on the cure conditions of a polydimethyl-siloxane (PDMS) elastomer; where both cure temperature and base-to-catalyst ratio were varied. The PDMS elastomer was evaluated as a bulk material and an impregnation matrix within a lightweight glass veil support. The E-glass support was selected for mechanical stiffness and dielectric strength. This work has shown a correlation between cure conditions and material physical properties. Tensile strength increased with cure temperature whereas breakdown voltage tended to be independent of process variations. The results will be used to direct material formulation based on specific insulation requirements.

insulation↗

In-situ Inspection of Reflowable-Interface Composite Joints During Cure in an Autoclave

In structural bonds, the interface between adherend and adhesive is nearly two-dimensional making it susceptible to minute quantities of contamination, which can cause weak bonds. Regulatory organizations such as the Federal Aviation Administration (FAA) often require redundant load paths in secondary-bonded, primary-structures to alleviate concerns with bonded performance. Under NASA’s Convergent Aeronautics Solutions (CAS) project, the Adhesive Free Bonding of Composites (AERoBOND) project is investigating reformulated aerospace epoxy-matrix resins to enable reflow and diffusion of the resin at the joint interface during a secondary bonding and cure process. The reflow and intermixing of the matrix resin during assembly can eliminate the material discontinuity at the interface, thereby removing the dependence of bond performance on adhesion at a nearly two-dimensional boundary. AERoBOND process development has evaluated a multitude of parameters including the materials used, the stoichiometric offset of the epoxy resins, time and temperature of cure, and thickness of each ply. Without in-situ process monitoring, the condition of a test article is unknown until mechanical testing is completed. This presentation describes the use of an in-situ ultrasonic inspection system to monitor the joining of two composite parts assembled using the AERoBOND technique. This work quantifies the elimination of the interface by measuring the wave reflection, or lack thereof, at the joint throughout the cure cycle. In addition, the results indicate when reflow and cure of the epoxy resin at the joint occurred. By using the recently developed in-situ inspection with a mobile ultrasonic transducer, localized results can be obtained across a large portion of the joint with high resolution.

Tyler B Hudson↗

In-situ Inspection of Reflowable-Interface Composite Joints During Cure in an Autoclave

In structural bonds, the interface between adherend and adhesive is nearly two-dimensional making it susceptible to minute quantities of contamination, which can cause weak bonds. Regulatory organizations such as the Federal Aviation Administration (FAA) often require redundant load paths in secondary-bonded, primary-structures to alleviate concerns with bonded performance. Under NASA’s Convergent Aeronautics Solutions (CAS) project, the Adhesive Free Bonding of Composites (AERoBOND) project is investigating reformulated aerospace epoxy-matrix resins to enable reflow and diffusion of the resin at the joint interface during a secondary bonding and cure process. The reflow and intermixing of the matrix resin during assembly can eliminate the material discontinuity at the interface, thereby removing the dependence of bond performance on adhesion at a nearly two-dimensional boundary. AERoBOND process development has evaluated a multitude of parameters including the materials used, the stoichiometric offset of the epoxy resins, time and temperature of cure, and thickness of each ply. Without in-situ process monitoring, the condition of a test article is unknown until mechanical testing is completed. This presentation describes the use of an in-situ ultrasonic inspection system to monitor the joining of two composite parts assembled using the AERoBOND technique. This work quantifies the elimination of the interface by measuring the wave reflection, or lack thereof, at the joint throughout the cure cycle. In addition, the results indicate when reflow and cure of the epoxy resin at the joint occurred. By using the recently developed in-situ inspection with a mobile ultrasonic transducer, localized results can be obtained across a large portion of the joint with high resolution.

Tyler B Hudson↗

In-situ Inspection of Reflowable-Interface Composite Joints During Cure in an Autoclave

In structural bonds, the interface between adherend and adhesive is nearly two-dimensional making it susceptible to minute quantities of contamination, which can cause weak bonds. Regulatory organizations such as the Federal Aviation Administration (FAA) often require redundant load paths in secondary-bonded primary-structures to alleviate the inability to certify bonded performance. To address this issue, the NASA Convergent Aeronautics Solutions (CAS): Adhesive Free Bonding of Composites (AERoBOND) project is investigating reformulated aerospace epoxy-matrix resins to enable reflow and diffusion of the resin at the joint interface during a secondary bonding and cure process. The reflow and intermixing of the matrix resin during assembly can eliminate the material discontinuity at the interface, thereby removing the dependence of bond performance on adhesion at a nearly two-dimensional boundary. AERoBOND process development has evaluated a multitude of parameters including the materials used, the stoichiometric offset of the epoxy resins, time and temperature of cure, and thickness of each ply. Without in-situ process monitoring, the condition of a test article is unknown until mechanical testing is completed. This paper describes the use of an in-situ ultrasonic inspection system to monitor the joining of two composite parts assembled using the AERoBOND technique. This work quantifies the interface by measuring the wave reflection, or lack thereof, at the joint throughout the cure cycle. In addition, the results indicate when reflow and cure of the epoxy resin at the joint occurred. By using the recently developed in-situ inspection method with a mobile ultrasonic transducer, localized results can be obtained across a large portion of the joint with high resolution.

Tyler B Hudson↗

Novel Fast Cure Silicone Inks for Single-Step, Support-Free 3D Printing of Tall, Overhanging, and High Aspect Ratio Structures

Silicone elastomers have a broad variety of applications, such as soft robotics, biomedical devices, and structural metamaterials. The extrusion-based method known as direct ink write (DIW) has enabled the production of additively manufactured silicone structures. However, this method is limited to manufacturing mostly planar or pseudo-3D structures. Due to the low self-supporting capabilities of extruded strands for traditional silicone-based “inks,” obtaining tall or overhanging structures, or structures comprised by thin walls is not feasible. Here, in this study, a novel Fast Cure silicone-based ink is demonstrated that enables manufacturing of complex 3D structures. The Fast Cure ink is a two-part mixture and silicone structures are produced by inline mixing and coextrusion of a part containing a catalyst (part A) and a part containing a crosslinker (part B). By the virtue of crosslinking, the extruded strands rapidly rigidize, increasing their self-supportive capacity. Hence, structures can be obtained with superior shape retention and previously unobtainable parts are realized that are tall, with aspect ratios higher than 3, and have overhanging features, achieving inclination angles smaller than 35° with respect to the printing plane. These minimal sag parts are achieved without requiring extra curing or mechanisms, support structures, or suspension baths.

36 MATERIALS SCIENCE↗

Measuring thermal curing induced shrinkage of material extrusion based additive manufacturing silicone elastomer lattices by X-ray computed tomography

Thermal curing induces shrinkage in material extrusion based additive manufacturing silicone elastomer samples, resulting in discrepancies between as printed and final geometries. Knowing the extent to which the samples change in shape and size allows us to make appropriate modifications to the printing design to better control the geometry of the samples. We present an X-ray computed tomography (CT) based approach to determine filament-level shrinkage due to thermal curing of silicone elastomer samples printed with direct ink writing (DIW). The approach relies on custom-designed build plates that are resistant to the elevated curing temperatures and that have sufficiently distinct X-ray absorption characteristics from the silicone elastomer to ensure adequate segmentation of the latter in X-ray imaging data. We implement the approach to evaluate shrinkage in DIW ‘log pile’ samples with three distinct strand arrangements and demonstrate of how filament-level information can be extracted from the X-ray CT data.

Additive manufacturing↗

B‐Staging and Crosslinking of Polycarbosilane at Room Temperature: Cure Mechanism and Properties

The viscosity of polycarbosilane (PCS) polymers is not advantageous for free forming. Various fillers and heat are used to obtain a formable paste. Due to the low yield stress, structures and preforms tend to slump or resin will flow out, especially during the curing of the polymer. B-staging of PCS allows for a more stable structure from room temperature until the full cure of the allyl groups occurs with heat. Additionally, hydrosilation is an effective means of crosslinking at room temperature and controlling viscosity. A network structure was formed in SMP-10 using silane and a vinyl-based crosslinker to bridge each polymer chain. Pt addition catalysts were added to enhance the increase in viscosity to make a lightly crosslinked gel to aid in thickening and forming and to improve the ceramic yield at 1000°C. In conclusion, this enables several options for controlling rheology and improving the properties of preceramic polymers to avoid slumping during curing.

inorganic polymers↗

Solventless Dual‐Cure Liquid Resins Via Circular Use of Phthalic Anhydride for Recyclable Composite Applications

Abstract Fiber‐reinforced composites (FRCs) possess a remarkable strength‐to‐weight ratio, making them ideal light‐weighing alternative materials of metals used in automotive, aerospace, and outdoor equipment applications, but their recycling is challenging. Chemically recyclable thermoset polymers can enable fiber recovery and reuse; however, challenges remain in the separation and purification of depolymerized small molecules for efficient polymer recycling. To this end, a series of liquid resins for chemically recyclable polymer networks is designed based on phthalic anhydride, a widely produced and inexpensive chemical. The straightforward sublimation of phthalic anhydride is leveraged to enable a simple and efficient separation process for polymer recycling. To liquefy phthalic anhydride, five mono‐acryloyl‐phthalates are synthesized to obtain stable liquid resins together with phthalic diglycidyl ester. These liquid resins undergo dual‐cure reactions that comprise photopolymerization of acrylate and, subsequently, heat‐mediated epoxy‐acid polymerization reactions. These liquid resins exhibit moderate viscosities (2600–6400 cP @ 22 °C), fast curing, and robust thermomechanical properties (T g s from 71 to 116 °C). It is demonstrated that hydrolysis of the dual‐cured polymers completes within 2 h at 80 °C, and direct sublimation produces phthalic anhydride with 82% yield. This resin system is expected to provide a cost‐competitive, highly efficient platform for recyclable FRCs.

Polymer Science↗

Effects of cleavable comonomer structure and crosslinker chemistry on the performance and deconstructability of frontally cured pDCPD composites

Reclaiming undamaged carbon fiber from thermoset composites requires chemical recycling methods that leverage complete deconstruction of the polymer matrix. Cleavable comonomers enable chemical recycling of poly(dicyclopentadiene) (pDCPD) composites, but current systems suffer from reduced glass transition temperature (T g ), limiting application. Here, we investigate the effect of cleavable comonomer loading and cleavable crosslinker chemistry on network formation, thermomechanical properties, and fiber recovery in frontally cured pDCPD composites. All formulations fully deconstructed in acid and recovered fibers ranged from pristine to variably contaminated depending on crosslinker chemistry. Reducing backbone-cleaving comonomer content and introducing cleavable crosslinkers raised composite T g to 126–138 °C compared to 105 °C previously reported in deconstructable pDCPD composites. Although the cleavable crosslinkers increased T g in unreinforced polymers to 150–160 °C, the fiber-reinforced composite T g remained lower due to under-curing and interactions between the crosslinkers and the fiber surface. Increasing polymerization initiator loading improved comonomer conversion and yielded a deconstructable composite with T g = 151 °C, approaching the performance of non-deconstructable pDCPD composites (T g = 161 °C). This work clarifies how cleavable comonomer and crosslinker chemistry governs curing, thermomechanical performance, and reclaimed reinforcement quality, and the results highlight the need for more robust cleavable comonomers to realize multigenerational composite materials without sacrificing thermomechanical performance.

Carbon fibers↗

Characterization of Temporal Changes of Interfacial Air Voids During Adhesive Curing and Bonding for Adhesively-Bonded Structures

This paper studied the evolution of air voids at the substrate-adhesive interface during the curing and bonding process of an epoxy-based adhesive between two glass substrates due to the sequence of adhesive placement, external pressure, and plasma treatment on substrates for bonding. The experimental results showed that a higher quantity of interfacial voids were generated during adhesive curing when the substrate was attached to the adhesive compared to when the adhesive was applied and distributed on the substrate. Such interfacial voids can be efficiently removed or reduced by applying slight pressure on the bonded structure during adhesive curing, or by leveraging plasma-treated substrates, as less reported in the literature. This work provided practical suggestions for preparing adhesive joints with minimized interfacial air voids to enhance bonding performance, particularly for dissimilar joints such as metal-CFRTP (carbon-fiber-reinforced thermoplastic polymer), as well as combinations with different types of polymer composites.

Qiao, Yao [BATTELLE (PACIFIC NW LAB)] (ORCID:00000↗

Improved cure method for single component silicone rubber

Water is incorporated in a carrier and then thoroughly mixed with the single component silicone rubber containing acetic anhydride as a curing agent. Because curing occurs with the water supplied internally, controlled curing is possible within a reasonable period of time, regardless of the thickness of the material.

Lippitt, M. W.↗

The effects of various cure cycles upon the viability of Bacillus subtillis var. niger spores within solid propellant.

Saturethane solid propellant was used in all tests. The spore inoculum was evenly distributed in the propellant. Samples weighing approximately 5 g were aseptically removed, placed into curing ovens, and exposed to cure temperatures. Initial tests were conducted at 82 and 93 C. Analysis of the obtained data indicated that the survivor curves were not linear. Exposure of the inoculated propellant samples to 93 C reduced the initial population to less than 0.01% in about 20 hours. At 82 C, approximately 168 hours were required for a similar reduction. Tests involving curing temperatures of 105 and 115 C were also conducted. It is pointed out that changes in the mechanism of spore inactivation due to chemical and physical changes in the propellant could account for the nonlinear survivor curves obtained.

Brewer, W. A.↗

One-step microwave foaming and curing

Process that combines microwave foaming and curing of polyimide precursors in single step produces fire-resistant foam slabs of much larger volume than has previously been possible. By adding selected conductive fillers to powder precursors and by using high-power microwave oven, foam slabs with dimensions in excess of 61 by 61 by 7.6 cm are made. Typical foaming and curing and curing time is 35 minutes in microwave oven with additional 1 to 2 hour postcure in conventional oven.

Gagliani, J.↗

Lower-curing-temperature PMR polyimides

Studies were performed to achieve a lower-curing-temperature PMR polyimide. The use of m-aminostyrene as the end-cap instead of the monoalkyl ester of 5-normbornene-2,3 dicarboxylic acid was investigated in typical PMR formulations. Model compound studies were also performed. Differential scanning calorimetry studies were performed on model compounds and neat resins to establish their melting and curing characteristics. The elevated temperature weight loss characteristics of neat resins and graphite fiber composites were determined. The room temperature and short-time 260 C (500 F) mechanical properties of the composites were also determined. The use of m-aminostyrene end-caps reduced the final cure temperature of PMR resins by about 55 C (100 F), but the composites prepared with these resins are limited to use temperatures of about 260 C (500 F).

Serafini, T. T.↗

Characterization of initial cure reactions in propargyl and nadic end capped model compounds

Imide model compounds containing propargyl and nadic groups were studied to obtain a fundamental understanding of the reaction of these groups attached to imide oligomers. The initial cure reactions were examined by a variety of characterization techniques including high pressure liquid chromatography, infrared spectroscopy, thermal analyses, and mass spectroscopy. The initial step in the cure of propargyl end capped model compounds probably involved the formation of a new terminal acetylenic group. Configurational changes involving endo/exo isomerism was found in the nadimide model compounds. Nadimide compounds heated in air and in nitrogen appeared to cure by different mechanisms.

Young, P. R.↗