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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↗

Ultrasonic Inspection During Autoclave Cure of Reflowable-Interface Composite Joints

In structural bonds, the interface between adherend and adhesive is nearly two-dimensional making the interface 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 due to uncertainty in bond 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 that can eliminate the material discontinuity at the interface. Implementing in-situ process monitoring enables assessing the bond quality during processing rather than waiting for post-fabrication mechanical testing to be completed. In this paper, an in-situ ultrasonic inspection system is used to monitor the joining of three composite laminates assembled using the AERoBOND technique. For each panel, the amplitude of the wave reflection at the joint was measured throughout the cure cycle. The results indicate the timing and extent of reflow and cure of the epoxy resin at the joint. Factors indicating end of cure were ascertained and a metric was developed to qualitatively predict acceptable mode-II fracture toughness based on the ultrasonic amplitude at the joint line during cure. In addition, since the inspection system scans an area of the joint, high-resolution localized results can be obtained across the joint.

Tyler B Hudson↗

Offset-Stoichiometric Reflowable Composite Bonding Method with Adhesive for Mitigating Strict Faying Surface Tolerances

Inherent susceptibility of adhesive bonds to miniscule quantities of contamination can cause undetectable weakened bonds. For this reason, the Federal Aviation Administration (FAA) places strict regulations on adhesively bonded joints in primary aircraft structures. To meet certification requirements aircraft manufactures resort to redundant load paths in the form of fasteners which inherently add weight to the structure and increase manufacturing time. In prior work, a secondary bonding technique called AERoBOND was developed, which utilized off-stoichiometric epoxymatrix resins to facilitate reflow and diffusion of the resin within the joint interface during a secondary bonding/cure process, thus achieving a bond similar to a co-cured joint. However, the AERoBOND process required tight spatial tolerances between the two parts being joined. This study examined the utilization of conventional adhesive with the AERoBOND method to act as a filler in the joint line, effectively reducing the need for tight tolerances on the joining parts and serving as a flexible alternative for existing manufacturing processes. Ultrasonic inspection, optical microscopy, and ASTM International standard tests were performed to analyze the joints for defects and to quantify the mode-I and mode-II interlaminar fracture toughness and short beam strength of the proposed methodology with varying manufacturing parameters. The comprehensive results indicate that the AERoBOND+ method with and without surface preparation performs comparably to co-cured and conventional, adhesively bonded joints when secondary cured in an autoclave with 791 kPa of pressure. As an example, the AERoBOND+ panel without surface preparation bonded with 791 kPa of pressure (referred to as AB+3 throughout paper) had a mode-I fracture toughness (G Ic ) of 0.643 kJ/m 2 and a mode-II fracture toughness (G IIc ) of 4.000 kJ/m 2 in the non-precracked condition and 4.218 kJ/m 2 in the precracked condition at the adhesive-to-prepreg interface. These results were 96%, 142%, and 217%, respectively, of a co-cured baseline panel (referred to as C1 throughout paper).

Composites↗

Latent Cure Epoxy Resins for Reliable Joints in Secondary-Bonded Composite Structures

In high-performance polymer matrix composite assemblies, adhesive bonding is generally superior to mechanical fastening in structural performance and manufacturing efficiency. However, adhesive bonds are susceptible to minute levels of contamination accumulated during assembly that can lead to unpredictable, weak bonds. Current methods of measuring bond strength are all destructive mechanical tests. To overcome these challenges, redundant load paths (e.g., mechanical fasteners) are often implemented in secondary-bonded, primary-structures, which can greatly reduce structural performance. This study investigated reformulated aerospace epoxy matrix resins with stoichiometric offset to inhibit cure of the matrix resin prior to assembly. Inhibited resins can reflow and mix across the joint interface, which eliminates the material discontinuity and forms a homogenous joint with reliable fracture properties. The goal of this study was to develop and demonstrate secondary composite assemblies that are mechanically and microscopically indistinguishable from a co-cured composite joint. This article describes the development of latent epoxy resins, the fabrication of test articles, and the mechanical properties measured from experimental joints compared with conventional, co-cured laminates. Methods of in-line quality control using and infrared spectroscopy and post-assembly forensics are also described. The final mode-II fracture toughness measured from precracked AERoBOND specimens was similar to that measured from co-cured laminates indicating that later cure epoxy materials could be a suitable replacement for secondary bonding.

Polymer-matrix composites (PMCs)↗

Modified Epoxy Matrix Resins for Reduced Dependence on Redundant Fasteners in Secondary-Bonded Composite Structures

In structural bonds, the interface between adherend and adhesive is nearly two-dimensional making it susceptible to minute quantities of contamination that can lead to weak bonds. No methods currently exist to measure the strength of an adhesive bond nondestructively. For these reasons, regulating organizations such as the Federal Aviation Administration (FAA) often require redundant load paths in secondary-bonded, primary-structures to achieve certification for civil transport aircraft. To meet this requirement, manufacturers commonly install redundant fasteners (~105 fasteners in a twin-aisle airframe with composite fuselage and wings), which add tremendous complexity, time and cost, and significantly reduce performance of the airframe. Under NASA’s Convergent Aeronautics Solutions (CAS) Program, 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 interface during a secondary bonding/cure process. The mixing process eliminates the material discontinuity at the interface, thereby removing the dependence of bond performance on adhesion across a nearly two-dimensional boundary. The AERoBOND interface is similar to the interlaminar region formed during a co-cure process, so joint performance depends on the cohesive properties of the matrix resin, which can be measured, inspected non-destructively, and certified for flight with fewer redundant fasteners. This presentation describes the ongoing development of stoichiometrically-offset epoxy resins to control the degree of cure in composite joints and enable interfacial mixing during secondary bonding/curing. Details on the resin formulation, laminate fabrication, and mechanical testing will also be presented. The precracked mode-II fracture toughness measured from preliminary AERoBOND joints was similar for joints fabricated with conventional epoxy matrix materials.

thermoset, hardener, prepreg, assembly↗

AERoBOND Project Summary

Under NASA’s Convergent Aeronautics Solutions (CAS) project, the Adhesive-Free Bonding of Complex Composites (AERoBOND) project investigated off-stoichiometric epoxy polymers for fast, reliable assembly of epoxy matrix composite structures. The project goal was to demonstrate feasibility of the AERoBOND joining method by demonstrating mechanical properties greater than 80% of conventional co-cured materials while reducing structure weight by 1%. The project consisted of three convergent research areas: material and process development, systems analysis, and material and process modeling. Material and process development was the largest component of AERoBOND with approximately 6 FTE and 1WYE of support to formulate and characterize new resins, prepare carbon fiber prepregs, fabricate laminates, measure mechanical properties, analyze failure results, and select material and process improvements. The systems analysis activity estimated the potential reduction in part count and aircraft weight by comparing models of composite wing boxes with no fasteners (co-cured structure), fasteners in major joints (co-cured stringers), and fasteners in all joints. The materials and process modeling activity included a molecular model of the AERoBOND materials system to predict mechanical properties of resins with offset stoichiometry and a process model to predict the effect of resin formulation and processing conditions on the extent of mixing and degree of cure in a finished joint. As the number of airline passenger trips doubles in the next 20 years (IATA/Tourism Economics Air Passenger Forecasts, April 2019), the increased demand for new commercial aircraft is now the single greatest technical challenge to the airframe manufacturing industry. To meet efficiency requirements, new aircraft must be fabricated primarily from high performance structural composites, but manufacturing processes are inherently slow with the largest bottleneck attributed to assembly and installation of fasteners (NASA/TM–2019-220428). Manufactures of commercial transport aircraft are compelled to install more than 100,000 redundant fasteners into bonded joints to prevent failures due to unpredictable weak bonds. In structural adhesive bonds, the interface between adherend and adhesive is nearly two-dimensional making it susceptible to minute quantities of contamination, which can cause weak bonds. Currently, bond strength assessment is only possible through destructive testing (i.e., breaking the joint). For these reasons, regulatory organizations such as the Federal Aviation Administration (FAA) often require redundant load paths in secondary-bonded, primary-structures to alleviate concerns with bond performance. The AERoBOND process enables reflow of matrix resin during assembly to eliminate the material discontinuity at the interface, thereby eliminating the dependence of mechanical performance on interfacial adhesion. The AERoBOND joint is equivalent to the interlaminar region obtained during a co-cure process, so joint performance depends on the cohesive properties of the matrix resin. Conventional co-cured structures, although too costly and complex for large-scale manufacturing, are trusted by manufacturers and regulators, and are certified for flight with few or no redundant fasteners.Systems analysis performed on a composite wing model at the scale of a single-aisle commercial transport aircraft indicated that >20,000 redundant fasteners per wing could be eliminated by implementing the AERoBOND joining method. A total weight reduction of 15% was predicted in a wing box by eliminating fasteners and thinning components that must no longer support localized fastener loads and accommodate fastener dimensions. Interlaminar shear fracture toughness measured by the end-notched flexure test was greater than 1 kJ/m2 (nearly 140% of the co-cured benchmark property), which is greatly in excess of the project goals for mechanical properties. Testing was planned to measure interlaminar tensile fracture toughness as well as interlaminar tensile and shear strengths using the same AERoBOND configuration, but was delayed due to closure of LaRC facilities during the COVID-19 pandemic. The AERoBOND process model is partially validated and available for experimental use. It allows the user to input AERoBOND process parameters such as material composition, laminate configuration, and cure cycle to predict the final cure state of the AERoBOND joint. A preliminary, multi-scale material model was developed to predict AERoBOND joint mechanical properties (stiffness and strength) based on the cure state of the joint provided by the process model. The timing for transition of this technology within NASA is excellent as NASA initiates new enduring projects to address composites manufacturing rate challenges. AERoBOND technology is well suited to AAVP/AATT objectives for rapid manufacturing of a composite wing. A minimal effort (1 FTE/$15k procurement/0 WYE) is proposed in FY21 to continue a minor mechanical testing effort and maintain a SAA with ASX composites to develop commercial quality prepreg material. An RFI with the composites industry is suggested to quantify the technology gap between the current TRL and the TRL needed for transition to industry. A moderate effort [3-4 FTE/$150k/1 WYE (~$115k)] is proposed in FY22 for the “high rate composites manufacturing” project currently in planning. The partnership with ASX Composites will be expanded to produce material for sub-element/element-scale “panel-off” activities. Industry partnerships with airframe manufacturers is an expected component to explore damage tolerance and environmental stability. Further development of multi-scale modeling tools (process model, meso-scale model, and molecular model) is planned to enhance and deliver tools for rapid manufacturing infusion.

Frank Louis Palmieri↗

Molecular Dynamics Investigation of the Structural and Mechanical Properties of Off-Stoichiometric Epoxy Resins

Molecular dynamic (MD) simulations were performed to compute the mechanical properties of off-stoichiometric epoxy resins as a function of hardener/epoxy mixture ratio (r). Properties were characterized in relation to their microscopic structures. Such resins have been used recently for adhesive-free bonding of large-scale composite structures using the co-curing-ply method. In this process, two partially precured composite panels with hardener-poor (HP) off-stoichiometric resins are coupled with ply(ies) of complementary hardener-rich (HR) formulations and then cured simultaneously. This bonding process has the potential to produce reliable and certifiable composite joints without the need for additional fasteners, which are often required for many conventional bonding methods because even small amounts of contamination can cause a weak bond. The reflow and mixing of the HP/HR resin in this bonding process result in a joint with no discernable interface that should not be susceptible to surface contamination. However, incomplete mixing of the two offset resins may result in chemical heterogeneity of the cured polymeric joint. Thus, different r values may be obtained across the joint. Classical MD simulations were performed to compute the Young’s modulus of polymers with different r values and correlate their properties to network structures. High stiffness was associated with molecular packing due to chemical crosslinking, leading to a single network structure. Moreover, the networks became denser as the ratio approached the stoichiometric value r = 1. Thus, the r = 1 systems were single clusters, with high stiffness, high molecular weight, and a high degree of crosslinking. Structural properties such as radius of gyration and mean square displacement were determined to investigate the variation in the stiffness with respect to r. This MD simulation study was validated with experimental measurements.

Chang Woon Jang↗

Solder Reflow Failures in Electronic Components During Manual Soldering

This viewgraph presentation reviews the solder reflow failures in electronic components that occur during manual soldering. It discusses the specifics of manual-soldering-induced failures in plastic devices with internal solder joints. The failure analysis turned up that molten solder had squeezed up to the die surface along the die molding compound interface, and the dice were not protected with glassivation allowing solder to short gate and source to the drain contact. The failure analysis concluded that the parts failed due to overheating during manual soldering.

Teverovsky, Alexander↗

Carbon Nanotube Bonding Strength Enhancement Using Metal "Wicking" Process

Carbon nanotubes grown from a surface typically have poor bonding strength at the interface. A process has been developed for adding a metal coat to the surface of carbon nano tubes (CNTs) through a wicking process, which could lead to an enhanced bonding strength at the interface. This process involves merging CNTs with indium as a bump-bonding enhancement. Classical capillary theory would not normally allow materials that do not wet carbon or graphite to be drawn into the spacings by capillary action because the contact angle is greater than 90 degrees. However, capillary action can be induced through JPL's ability to fabricate oriented CNT bundles to desired spacings, and through the use of deposition techniques and temperature to control the size and mobility of the liquid metal streams and associated reservoirs. A reflow and plasma cleaning process has also been developed and demonstrated to remove indium oxide, and to obtain smooth coatings on the CNT bundles.

Lamb, James L.↗

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.↗