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At least 127 records · Page 7

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↗

RF cured nanocomposite adhesives for multi-material joining applications

A method for fabricating, and curing, nanocomposite adhesives including introducing nanoheater elements into a heat-curing adhesive to fabricate a nanocomposite adhesive, and providing a radio-frequency (RF) electromagnetic wave to the nanocomposite adhesive to heat, and cure the nanocomposite adhesive. The nanocomposite adhesive is physically applied to first and second materials to bond the first and second materials upon curing of the nanocomposite adhesive, and the RF electromagnetic wave has a frequency in the radio-frequency range, having energy that is transferred to the nanoheater elements by electromagnetic wave interactions with permanent and induced dipoles, intrinsic photon-phonon interaction, or interactions with nanoheater defects and grain structures.

Zhang, Yuepeng↗

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↗

Manufacturing and characterization of a boron-loaded fast-cured plastic organic scintillator

A novel fast-cured, boron-loaded, plastic organic scintillator was developed and characterized. A diisopropylnaphthalene-containing scintillator was manufactured in minutes with the addition of two commercially available fast-curing monomers, isobornyl acrylate (IBOA) and 1,6-Hexanediol dimethacrylate (HDDMA). Further, the light yield of the device was measured to be approximately 70% relative to a similarly sized, but several-year-aged, EJ-276 detector. Using a coincidence capture technique, the neutron capture light output was found to be 87.7 ± 4.2 keVee, which was 1.47 ± 0.07 greater than the light output from a 59.5 keV electron. Producing a viable fast-cured and thermal-neutron-sensitive detector enables the capability to pursue cost-effective 3D printed thermal neutron detectors in a timely manner.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

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↗

Elucidating Diiodomethane-Induced Improvement in Photonically Cured MAPbI 3 Solar Cells

Diiodomethane (CH 2 I 2 ) has been reported to improve the photonically cured perovskite solar cell (PSC) device performance by reducing pinholes. Here we show that even for pinhole-free methylammonium lead iodide (MAPbI 3 ) made by photonic curing, adding CH 2 I 2 promotes significant performance improvement. We elucidate the mechanisms behind the observed improvement. In addition to current-density versus voltage measurements, we perform a wide variety of characterization to compare the crystallinity, grain structure, optical, chemical, and electrical properties of the photonically cured samples with and without CH 2 I 2 in the MAPbI 3 layer to those of thermally annealed devices. Here, the addition of CH 2 I 2 promotes grain growth in the vertical direction, increases the I/Pb ratio in the final film, and removes the I - ionic diffusion and defect signature associated with iodine interstitials. As a result, we achieve a champion efficiency of 15.04% with MAPbI 3 conversion time of 20 ms, comparable to PSCs that have MAPbI 3 layer thermally annealed for 10 min. Understanding the mechanisms behind additive-induced improvements for non-thermal annealing processes is critical to enabling high-speed PSC manufacturing.

14 SOLAR ENERGY↗

Photonic curing of solution-deposited ZrO 2 dielectric on PEN: a path towards high-throughput processing of oxide electronics

High-throughput manufacturing of oxide electronics will enable new applications ranging from large-area displays to flexible medical devices and low-cost solar panels. However, high quality oxide films from solution-based precursors typically require 20 minutes or more of thermal annealing at high temperature (> 250 °C) for each layer, severely limiting both the throughput and substrate choice. Here, we report high speed photonic curing of ZrO 2 dielectric thin films on flexible plastic substrates. The curing and patterning processes can be achieved simultaneously by using shadow mask patterning or adjusting conditions to convert oxide only on top of underlying metal contacts, i.e. self-aligned patterning. Metal-insulator-metal capacitors using two layers of ZrO 2 films photonically cured in just 100 seconds per layer show non-dispersive capacitance-frequency behavior from 10 2 to 10 6 Hz, high areal capacitance of 200 nF/cm 2 and low dissipation factor of 0.03 at 10 5 Hz, leakage current density of ~ 10 -7 A/cm 2 at an applied field of 2 MV/cm, and a breakdown field of nearly 8 MV/cm. Using an upgraded tool, similar dielectric properties are achieved in as short as 100 milliseconds using a single pulse of light, revealing a pathway to oxide film processing beyond 30 m/min.

14 SOLAR ENERGY↗

Atomic force microscopy and scanning electron microscopy characterization of the controlling of surface morphology of epoxy‐amine‐cured spin‐coated films

Abstract Atomic force microscopy (AFM) was successfully used to study spin‐coated, amine‐cured epoxy film microstructure and morphology. The air‐epoxy and epoxy‐substrate interfaces were examined using tapping‐mode height and phase imaging AFM. The impact of relative humidity on the morphology and microstructure of the surfaces was determined. AFM was able to elucidate the changes on the surface as relative humidity during processing increased. It was observed that large nodular formations formed on the epoxy surface expose to the air but not epoxy surface formed on the substrate in addition to varying regions of more or less compliant structures, which was attributed to carbamate formation caused by the amine curing agent reaction with atmospheric CO 2 . Scanning electron microscopy (SEM) was used to further elucidate interface and interphase morphology of spin‐coated epoxies. Experimentation also demonstrated that post‐curing above the glass transition did not change the morphology structure, suggesting surface structures are “locked‐in.” SEM was used to further elucidate how the interface and interphase change with changing environmental conditions at both the air‐epoxy and epoxy‐substrate interface/interphases, including the impact of atmospheric CO 2 on Marangoni cell formation.

Shenk, Timothy M.↗

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↗

Plastic shrinkage of mortars cured with a paraffin-based compound – Bimodal neutron/X-ray tomography study

Early-age drying (immediately after casting) of mortars and the corresponding plastic shrinkage were studied using bimodal neutron/X-ray computed tomography. This novel, correlative 3D imaging mode enabled studying simultaneously and without any source of spurious perturbation the water migration and loss processes together with the corresponding deformations due to plastic shrinkage. Bimodal imaging opens up new possibilities for studying dynamic processes of coupled water transport and deformations in porous solids. The measurements were carried out on model systems (cylindrical mortar specimens with height of 19 mm). The study focused on the effect of a paraffin-based curing compound. Our results confirm that when the curing compound was applied directly onto the drying surface in a sufficient amount, both the evaporation rate and the rate of vertical displacement (settlement) were substantially reduced. The results shed a new light on the mechanisms of plastic shrinkage and the action of curing compounds.

36 MATERIALS SCIENCE↗

Influence of curing temperature on belite cement hydration: A comparative study with Portland cement

Belite cements (BCs) could be a more sustainable binder than Portland cements (PCs) but adequate knowledge of the hydration features has still to be built. In particular, the mild curing hydration temperature effects have been extensively studied for PCs but not for BCs. This research was triggered by a previous work reporting improved mechanical strengths of BCs at higher curing temperatures. Here, we report the hydration characteristics of a BC at 20, 40 and 60 °C and compared to those of a typical PC. We have corroborated previous findings and used a multi-technique approach including Rietveld phase analysis, thermal analysis, calorimetry, silicon MAS-NMR, mercury intrusion porosimetry and chiefly synchrotron X-ray microtomography, to thoroughly understand the different behavior. In a nutshell, the improved mechanical performances at mild curing temperatures for BCs are mainly due to a much larger belite degree of reaction, with lower porosity coarsening of belite cements also playing a role.

36 MATERIALS 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↗

Photonic Curing Enabling High-Speed Processing for Perovskite Solar Cells

The thermal annealing step is the bottleneck to high-throughput manufacturing of perovskite solar cells. In this work, we investigate photonic curing to replace thermal annealing for the sol gel NiO hole transport layer. Using solar cell device current density-voltage performance as a metric, we compare the effects of thermal annealing and photonic curing on the conversion of sol gel NiO films deposited on top of indium tin oxide coated Willow® glass substrates. The significant reduction in processing time validates photonic curing as the enabling tool for high-speed manufacturing.

Xu, Weijie↗

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↗