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DOE OSTI2021

Crossover from hydrogen to chemical bonding

Hydrogen bonds (H-bonds) can be interpreted as a classical electrostatic interaction or as a covalent chemical bond if the interaction is strong enough. As a result, short strong H-bonds exist at an intersection between qualitatively different bonding descriptions, with few experimental methods to understand this dichotomy. The [F-H-F] − ion represents a bare short H-bond, whose distinctive vibrational potential in water is revealed with femtosecond two-dimensional infrared spectroscopy. It shows the superharmonic behavior of the proton motion, which is strongly coupled to the donor-acceptor stretching and disappears on H-bond bending. In combination with high-level quantum-chemical calculations, we demonstrate a distinct crossover in spectroscopic properties from conventional to short strong H-bonds, which identify where hydrogen bonding ends and chemical bonding begins.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Experimental and theoretical insights into the effects of pH on catalysis of bond-cleavage by the lignin peroxidase isozyme H8 from Phanerochaete chrysosporium

Abstract Background Lignin peroxidases catalyze a variety of reactions, resulting in cleavage of both β-O-4′ ether bonds and C–C bonds in lignin, both of which are essential for depolymerizing lignin into fragments amendable to biological or chemical upgrading to valuable products. Studies of the specificity of lignin peroxidases to catalyze these various reactions and the role reaction conditions such as pH play have been limited by the lack of assays that allow quantification of specific bond-breaking events. The subsequent theoretical understanding of the underlying mechanisms by which pH modulates the activity of lignin peroxidases remains nascent. Here, we report on combined experimental and theoretical studies of the effect of pH on the enzyme-catalyzed cleavage of β-O-4′ ether bonds and of C–C bonds by a lignin peroxidase isozyme H8 from Phanerochaete chrysosporium and an acid stabilized variant of the same enzyme. Results Using a nanostructure initiator mass spectrometry assay that provides quantification of bond breaking in a phenolic model lignin dimer we found that catalysis of degradation of the dimer to products by an acid-stabilized variant of lignin peroxidase isozyme H8 increased from 38.4% at pH 5 to 92.5% at pH 2.6. At pH 2.6, the observed product distribution resulted from 65.5% β-O-4′ ether bond cleavage, 27.0% C α -C 1 carbon bond cleavage, and 3.6% C α -oxidation as by-product. Using ab initio molecular dynamic simulations and climbing-image Nudge Elastic Band based transition state searches, we suggest the effect of lower pH is via protonation of aliphatic hydroxyl groups under which extremely acidic conditions resulted in lower energetic barriers for bond-cleavages, particularly β-O-4′ bonds. Conclusion These coupled experimental results and theoretical explanations suggest pH is a key driving force for selective and efficient lignin peroxidase isozyme H8 catalyzed depolymerization of the phenolic lignin dimer and further suggest that engineering of lignin peroxidase isozyme H8 and other enzymes involved in lignin depolymerization should include targeting stability at low pH.

09 BIOMASS FUELS↗

DOE OSTI2022

Fine Pitch Bonding for High Density Interconnects

CTE (coefficient of thermal expansion) mismatch between two wafers has potential for brittle failure when large areas are bonded on top of one another (wafer to wafer or wafer to die bonds). To address this type of failure, we proposed patterning a polymer around metallic interconnects. For this project, utilized benzo cyclobutene (BCB) to form the bond and accommodate stress. For the metal interconnects, we used indium. To determine the benefits of utilizing BCB, mechanical shear testing of die bonding with just BCB were compared to die bonded just with oxide. These tests demonstrated that BCB, when cured for only 30 minutes and bonded at 200°C, the BCB was able to withstand shear forces similar to oxide. Furthermore, when the BCB did fail, it experienced a more ductile failure, allowing the silicon to crack, rather than shatter. To demonstrate the feasibility of using BCB between indium interconnects, wafers were pattered with layers of BCB with vias for indium or ENEPIG (electroless nickel, electroless palladium, immersion gold). Subsequently, these wafers were pattered with a variety of indium or ENEPIG interconnect pitches, diameters, and heights. These dies were bonded under a variety of conditions, and those that held a bond, were cross-sectioned and imaged. Images revealed that certain bonding conditions allow for interconnects and BCB to achieve a void-less bond and thus demonstrate that utilizing polymers in place of oxide is a feasible way to reduce CTE stress.

36 MATERIALS SCIENCE↗

NASA NTRS1975

High reliability bond program using small diameter aluminum wire

The program was undertaken to characterize the performance of small diameter aluminum wire ultrasonically bonded to conductors commonly encountered in hybrid assemblies, and to recommend guidelines for improving this performance. Wire, 25.4, 38.1 and 50.8 um (1, 1.5 and 2 mil), was used with bonding metallization consisting of thick film gold, thin film gold and aluminum as well as conventional aluminum pads on semiconductor chips. The chief tool for evaluating the performance was the double bond pull test in conjunction with a 72 hour - 150 C heat soak and -65 C to +150 C thermal cycling. In practice the thermal cycling was found to have relatively little effect compared to the heat soak. Pull strength will decrease after heat soak as a result of annealing of the aluminum wire; when bonded to thick film gold, the pull strength decreased by about 50% (weakening of the bond interface was the major cause of the reduction). Bonds to thin film gold lost about 30 - 40% of their initial pull strenth; weakening of the wire itself at the bond heel was the predominant cause. Bonds to aluminum substrate metallization lost only about 22%. Bonds between thick and thin film gold substrate metallization and semiconductor chips substantiated the previous conclusions but also showed that in about 20 to 25% of the cases, bond interface failure occurred at the semiconductor chip.

Macha, M.↗

NASA NTRS1985

Solid-state Bonding of Superplastic Aluminum Alloy 7475 Sheet

Experimental works were carried out to study the feasibility of solid state bonding of superplastic aluminum 7475 sheet. Amount of deformation, bonding time, surface cleaning method and intermediate layer were the process parameters investigated. Other parameters, held constant by the superplastic forming condition which is required to obtain a concurrent solid state bonding, are bonding temperature, bonding pressure and atmosphere. Bond integrity was evaluated through metallographic examination, X-ray line scan analysis, SEM fractographic analysis and lap shear tests. The early results of the development program indicated that sound solid state bonding was accomplished for this high strength 7475 alloy with significant amounts of deformation. A thin intermediate layer of the soft 5052 aluminum alloy aided in achieving a solid state bonding by reducing the required amount of plastic deformation at the interface. Bond strength was substantially increased by a post bond heat treatment.

Byun, T. D. S.↗

NASA NTRS1988

Evaluation of a thermoplastic polyimide (422) for bonding GR/PI composite

A hot-melt processable copolyimide previously studied and characterized as an adhesive for bonding Ti-6Al-4V was used to bond Celion 6000/LARC-160 composite. Comparisons are made for the two adherend systems. A bonding cycle was determined for the composite bonding and lap shear specimens were prepared which were thermally exposed in a forced-air oven for up to 5000 h at 204 C. The lap shear strengths (LSSs) were determined at RT, 177, and 204 C. After thermal exposure at RT, 177, and 204 C the LSS decreased significantly; however, a slight increase was noted for the 204 C tests. Initially the LSS values are higher for the bonded Ti-6Al-4V than for the bonded composite, however, the LSS decreases dramatically between 5000 and 10,000 h of 204 C thermal exposure. Longer periods of thermal exposure up to 20,000 h results in further decreases in the LSSs. Although the bonded composite retained useful strengths for exposures up to 5000 h, based on the poor results of the bonded Ti-6Al-4V beyond 5000 h, the 422 adhesive bonded composites would most likely also produce poor strengths beyond 5000 h exposure. Adhesive bonded composite lap shear specimens exposed to boiling water for 72 h exhibited greatly reduced strengths at all test temperatures. The percent retained after water boil for each test temperature was essentially the same for both systems.

Progar, Donald J.↗

NASA NTRS1989

A noncontacting scanning photoelectron emission technique for bonding surface cleanliness inspection

Molecular contamination of bonding surfaces can drastically affect the bond strength that can be achieved and therefore the structural integrity and reliability of the bonded part. The presence of thin contaminant films on bonding surfaces can result from inadequate or incomplete cleaning methods, from oxide growth during the time between cleaning (such as grit blasting) and bonding, or from failure to properly protect cleaned surfaces from oils, greases, fingerprints, release agents, or deposition of facility airborne molecules generated by adjacent manufacturing or processing operations. Required cleanliness levels for desired bond performance can be determined by testing to correlate bond strength with contaminant type and quantity, thereby establishing the degree of contamination that can be tolerated based on the strength that is needed. Once the maximum acceptable contaminant level is defined, a method is needed to quantitatively measure the contaminant level on the bonding surface prior to bonding to verify that the surface meets the established cleanliness requirement. A photoelectron emission technique for the nondestructive inspection of various bonding surfaces, both metallic and nonmetallic, to provide quantitative data on residual contaminant levels is described. The technique can be used to scan surfaces at speeds of at least 30 ft/min using a servo system to maintain required sensor to surface spacing. The fundamental operation of the photoelectron emission sensor system is explained and the automated scanning system and computer data acquisition hardware and software are described.

Gause, Raymond L.↗

NASA NTRS1988

Evaluation of a thermoplastic polyimide (422) for bonding GR/PI composite

A hot-melt processable copolyimide previously studied and characterized as an adhesive for bonding Ti-6Al-4V was used to bond Celion 6000/LARC-160 composite. Comparisons are made for the two adherend systems. A bonding cycle was determined for the composite bonding and lap shear specimens were prepared which were thermally exposed in a forced-air oven for up to 5000 h at 204 C. The lap shear strengths (LSSs) were determined at RT, 177, and 204 C. After thermal exposure at RT, 177, and 204 C the LSS decreased significantly; however, a slight increase was noted for the 204 C tests. Initially the LSS values are higher for the bonded Ti-6Al-4V than for the bonded composite, however, the LSS decreases dramatically between 5000 and 10,000 h of 204 C thermal exposure. Longer periods of thermal exposure up to 20,000 h results in further decreases in the LSSs. Although the bonded composite retained useful strengths for exposures up to 5000 h, based on the por results of the bonded Ti-6Al-4V beyond 5000 h, the 422 adhesive bonded composites would most likely also produce poor strengths beyond 5000 h exposure. Adhesive bonded composite lap shear specimens exposed to boiling water for 72 h exhibited greatly reduced strengths at all test temperatures. The percent retained after water boil for each test temperature was essentially the same for both systems.

Progar, Donald J.↗

NASA NTRS1991

Evaluation of Surlyn 8920 as PHE Visor Material and Evaluations of New Adhesives for Improving Bonding Between Teflon and Stainless Steel at Cryogenic Temperature

Two studies are presented, and in the first study, Surlyn 8920 (an ionic and amorphous low density polyethylene made by Dupont) was evaluated as a possible replacement of Plexyglass G as PHE visor material. Four formulations of the polymer were made by adding different amounts of UV stabilizer, energy quencher, and antioxident in a Brabender Plasticorder. The formulated polymers were molded in the form of sheets in a compression molder. Cut samples from the molded sheets were exposed in a weatherometer and tested on Instron Tensile Tester for strength and elongation. Specially molded samples of the formulated polymers were subjected to Charpy Impact Tests. In the second study, preliminary evaluations of adhesives for improvement of bonding between Teflon and stainless steel (SS) were performed. Kapton, a high temperature polyimide made by Dupont, and a rubber based adhesive made by Potter Paint Co., were evaluated against industrial quality epoxy, the current material used to bond Teflon and SS. The degreased surfaces of the SS discs were etched mechanically, with a few of these etched chemically. The surfaces of the SS discs were etched mechanically, with a few of these etched chemically. Bonding strengths were evaluated using lap shear tests on the Instron Tensile Tester for the samples bonded by Kapton and industrial quality epoxy. Bond strengths were also evaluated using a pull test on the Instron for the samples bonded by Potter adhesive (CWL-152) and industrial quality epoxy. Based on limited lap shear data, Kapton gave bond strength favorable compared to that of industrial epoxy. Based on limited pull test data, Kapton bonded and CWL-152 bonded samples showed poor strength compared to epoxy bonded sample.

Ray, Asit K.↗

NASA NTRS1997

Nondestructive Evaluation of Adhesively Bonded Joints by Acousto-Ultrasonic Technique and Acoustic Emission

Reliable applications of adhesively bonded joints require an effective nondestructive evaluation technique for their bond strength prediction. To properly evaluate factors affecting bond strength, effects of defects such as voids and disbonds on stress distribution in the overlap region must be understood. At the same time, in order to use acousto-ultrasonic (AU) technique to evaluate bond quality, the effect of these defects on dynamic response of single lap joints must be clear. The stress distribution in a single lap joint with and without defects (void or disbond) is analyzed. A bar-Theta parameter which contains adherend and adhesive thickness and properties is introduced. It is shown for bonded joints with bar-Theta greater than 10, that a symmetric void or disbond in the middle of overlap up to the 70 percent of overlap length has negligible effect on bond strength. In contrast frequency response analyses by a finite element technique showed that the dynamic response is affected significantly by the presence of voids or disbonds. These results have direct implication in the interpretations of AU results. Through transmission attenuation and a number of AU parameters for various specimens with and without defects are evaluated. It is found that although void and disbond have similar effects on bond strength (stress distribution), they have completely different effects on wave propagation characteristics. For steel-adhesive-steel specimens with voids, the attenuation changes are related to the bond strength. However, the attenuation changes for specimens with disbond are fairly constant over a disbond range. In order to incorporate the location of defects in AU parameters, a weighting function is introduced. Using an immersion system with focused transducers, a number of AU parameters are evaluated. It is found that by incorporating weighting functions in these parameters better sensitivities (AU parameters vs. bond strength) are achieved. Acoustic emission (AE) activities of steel-adhesive-steel specimens with bar-Theta equal to 3.4 are monitored. Two different formats of energy vs. time have resulted, each corresponding to the perfect specimens or the specimens with void or disbond. The relative acoustic energy and the number of events at failure are found to be a means for predicting the bond strength.

Nayeb-Hashemi, Hamid↗

NASA NTRS1998

A 90 GHz Amplifier Assembled Using a Bump-Bonded InP-Based HEMT

We report on the performance of a novel W-band amplifier fabricated utilizing very compact bump bonds. We bump-bonded a high-speed, low-noise InP high electron mobility transistor (HEMT) onto a separately fabricated passive circuit having a GaAs substrate. The compact bumps and small chip size were used for efficient coupling and maximum circuit design flexibility. This new quasi-monolithic millimeter-wave integrated circuit (Q-MMIC) amplifier exhibits a peak gain of 5.8 dB at approx. 90 GHz and a 3 dB bandwidth of greater than 25%. To our knowledge, this is the highest frequency amplifier assembled using bump-bonded technology. Our bump-bonding technique is a useful alternative to the high cost of monolithic millimeter-wave integrated circuits (MMIC's). Effects of the bumps on the circuit appear to be minimal. We used the simple matching circuit for demonstrating the technology - future circuits would have all of the elements (resistors, via holes, bias lines, etc.) included 'in conventional MMIC's. Our design in different from other investigators' efforts in that the bumps are only 8 microns thick by 15 microns wide. The bump sizes were sufficiently small that the devices, originally designed for W-band hybrid circuits, could be bonded without alteration. Figure 3 shows the measured and simulated magnitude of S-parameters from 85-120 GHz, of the InP HEMT bump-bonded to the low noise amplifier (LNA) passive. The maximum gain is 5.8 dB at approx. 90 GHz, and gain extends to 117 GHz. Measurement of a single device (without matching networks) shows approx. 1 dB of gain at 90 GHz. The measured gain of the amplifier agrees well with the design in the center of the measurement band, and the agreement falls off at the band edges. Since no accommodation for the bump-bonding parasitics was made in the design, the result implies that the parasitic elements associated with the bonding itself do not dominate the performance of the LNA circuit. It should be noted that this amplifier was designed for good noise performance, which is why the input and output return losses are poorer than one would expect for an amplifier simply matched for gain. However, noise performance has not been measured at this time. While the agreement between modeled vs. experimental data is not exact, the data prove that bump-bonded technology can be used for amplifiers at frequencies at least as high as 100 GHz. JPL is pursuing this technology as a way to economically and quickly incorporate the best available HEMTs into a circuit with all of the reliability and circuit design flexibility offered by MMIC technology. We are currently using the technology to fabricate 4-stage, wide-band, W-band LNA's. We have also performed pull and shear tests which show that the bump bonds are sufficiently robust for any anticipated application.

Pinsukanjana, Paul R.↗

NASA NTRS2007

Fabrication and Characterization of Diffusion Bonds for Silicon Carbide

Diffusion bonds of silicon carbide (SiC) were fabricated using several different types of titanium (Ti) based interlayers between the SiC substrates. The interlayers were an alloyed Ti foil, a pure Ti foil, and a physically vapor deposited (PVD) Ti coating. Microscopy was conducted to evaluate the cross-sections of the resulting bonds. Microprobe analysis identified reaction formed phases in the diffusion bonded region. Uniform and well adhered bonds were formed between the SiC substrates. In the case where the alloyed Ti foil or a thick Ti coating (i.e. 20 micron) was used as the interlayer, microcracks and several phases were present in the diffusion bonds. When a thinner interlayer was used (i.e. 10 micron PVD Ti), no microcracks were observed and only two reaction formed phases were present. The two phases were preferred and fully reacted phases that did not introduce thermal stresses or microcracks during the cool-down stage after processing. Diffusion bonded samples were evaluated with the non-destructive evaluation (NDE) methods of pulsed thermography and immersion ultrasonic testing. Joined SiC substrates that were fully bonded and that had simulated bond flaws in the interlayer were also evaluated using immersion ultrasound. Pull testing was conducted on the bonds to determine the tensile strength. To demonstrate the joining approach for a complex multilayered component for a low NOx injector application, the diffusion bonding approach was used to join three 4" diameter SiC discs that contained complex fuel and air flow channels.

Halbig, Michael↗

NASA NTRS2008

Evaluation of the Effect of Silicone Contamination on Various Bond Systems and the Feasibility of Removing the Contamination

Silicone is a contaminant that can cause catastrophic failure of a bond system depending on the materials and processes used to fabricate the bond system. Unfortunately, more and more materials are fabricated using silicone. The purpose of this testing was to evaluate which bond systems are sensitive to silicone contamination and whether or not a cleaning process could be utilized to remove the silicone to bring the bond system performance back to baseline. Due to the extensive nature of the testing, attempts will be made to generalize the understanding within classes of substrates, bond systems, and surface preparation and cleaning methods. This study was done by contaminating various metal (steel, Inconel, and aluminum), phenolic (carbon-cloth phenolic [CCP] and glass-cloth phenolic [GCP]), and rubber (natural rubber, asbestos-silicone dioxide filled natural butyldiene rubber [ASNBR]; silica-filled ethylene propylenediene monomer [SFEPDM], and carbon-filled ethylene propylenediene monomer [CFEPDM]) substrates which were then bonded using various adhesives and coatings (epoxy-based adhesives, paints, ablative compounds, and Chemlok adhesives) to determine the effect silicone contamination has on a given bond system's performance. The test configurations depended on the bond system being evaluated. The study also evaluated the feasibility of removing the silicone contamination by cleaning the contaminated substrate prior to bonding. The cleaning processes also varied depending on bond system.

Stanley, Stephanie D.↗

NASA NTRS2008

Evaluation of the Effect of Silicone Contamination on Various Bond Systems and the Feasibility of Removing the Contamination

Silicone is a contaminant that can cause catastrophic failure of a bond system depending on the materials and processes used to fabricate the bond system, Unfortunately, more and more materials are fabricated using silicone. The purpose of this testing was to evaluate which bond systems are sensitive to silicone contamination and whether or not a cleaning process could be utilized to remove the silicone to bring the bond system performance back to baseline. Due to the extensive nature of the testing attempts will be made to generalize the understanding within classes of substrates, bond systems, and surface preparation and cleaning methods. This study was done by contaminating various meta! (steel, inconel, and aluminum), phenolic (carbon cloth phenolic and glass cloth phenolic), and rubber (natural rubber, asbestos-silicone dioxide filled natural butyldiene rubber, silica-filled ethylene propylenediene monomer, and carbon-filled ethylene propylenediene monomer) substrates which were then bonded using various adhesives and coatings (epoxy-based adhesives, paints, ablative compounds, and Chemlok adhesives) to determine the effect silicone contamination has on a given bond system's performance. The test configurations depended on the bond system being evaluated. The study also evaluated the feasibility of removing the silicone contamination by cleaning the contaminated substrate prior to bonding. The cleaning processes also varied depending on bond system.

Stanley, Stephanie D.↗

NASA NTRS2016

Nondestructive Evaluation of Adhesive Bonds via Ultrasonic Phase Measurements

The use of advanced composites utilizing adhesively bonded structures offers advantages in weight and cost for both the aerospace and automotive industries. Conventional nondestructive evaluation (NDE) has proved unable to reliably detect weak bonds or bond deterioration during service life conditions. A new nondestructive technique for quantitatively measuring adhesive bond strength is demonstrated. In this paper, an ultrasonic technique employing constant frequency pulsed phased-locked loop (CFPPLL) circuitry to monitor the phase response of a bonded structure from change in thermal stress is discussed. Theoretical research suggests that the thermal response of a bonded interface relates well with the quality of the adhesive bond. In particular, the effective stiffness of the adhesive-adherent interface may be extracted from the thermal phase response of the structure. The sensitivity of the CFPPLL instrument allows detection of bond pathologies that have been previously difficult-to-detect. Theoretical results with this ultrasonic technique on single epoxy lap joint (SLJ) specimens are presented and discussed. This technique has the potential to advance the use of adhesive bonds - and by association, advanced composite structures - by providing a reliable method to measure adhesive bond strength, thus permitting more complex, lightweight, and safe designs.

Haldren, Harold A.↗

NASA NTRSDate not supplied

Measurement System Analysis of a Novel Phase-Based Ultrasonic NDE Technique for Bond Strength Measurement

Fiber reinforced polymer parts have shown tremendous benefits in aerospace structural applications, but their qualification and certification for use in safety critical areas are currently hindered by the lack of a capable non-destructive evaluation (NDE) method or technique for the inspection of these adhesively bonded parts. Conventional NDE methods and techniques typically detect gross bond defects in a qualitative (Pass/Fail) manner. These techniques struggle to detect weak or kissing bonds. Also, there are no widely adopted NDE methods or techniques for measuring interfacial bond strength or detecting kissing bonds. Bond strength is currently ensured by process control and semi-destructive testing. Results from recent research from other authors, including but not limited to mechanical testing, have shown an excellent correlation between interfacial stiffness of an adhesively bonded joint and the adhesive bond strength of that joint. In this paper, a measurement system analysis (MSA) of a novel phase-based ultrasonic NDE Technique, developed at NASA Langley Research Center, is presented for bond strength measurement to assess at an increased level the measurement process and identify components of variation in that measurement process.

Ultrasound↗

DOE OSTI2026

Chemical bonding, phase stability and magnetic property in Sm 2 Fe 17 X 3 (X=H, C, N): A first-principles perspective

As a promising alternative to Nd–Fe–B magnets, the critical rare earth free Sm 2 Fe 17 X 3 (X = C, N) exhibits potential for high-performance magnets. However, their poor phase stability remains a major obstacle to developing bulk magnets. We investigated the phase stability and intrinsic magnetic properties of Sm 2 Fe 17 X 3 (X = H, C, N) using first-principles calculations and chemical bond analysis. The formation energies are negative, while the decomposition energies are −1.53, 0.348, and −0.74 eV per formula unit for X = H, C, and N, respectively, which is responsible for the weak thermal stability. Our chemical bond analysis reveals that the bonding asymmetry between Sm–X and Fe–X interactions creates local structural distortions and degrades the phase stability of Sm 2 Fe 17 X 3 . The project Crystal Orbital Hamilton Population (-pCOHP) analysis indicates that the Sm–X bonding remains positive up to the Fermi level, indicating stable bonding interactions. Here, in contrast, the Fe–X bonding becomes negative near the Fermi level, signifying anti-bonding contributions that reduce structural stability. Interstitial atoms X expand the lattice and enhance Fe magnetic moments, but Fe–X bonding suppresses neighboring Fe moments. Electron transfer from Sm to X modifies the valence state of Sm and the crystal field at the site, contributing to enhanced magnetocrystalline anisotropy in Sm 2 Fe 17 X 3 . Among the interstitial elements, carbon and nitrogen—with their larger atomic radius and higher electronegativity—induce greater lattice expansion and form stronger bonds with neighboring Sm and Fe atoms compared to hydrogen. Consequently, Sm 2 Fe 17 X 3 (X = C and N) exhibits better phase stability and significant improvement in magnetic properties.

Chemical bonding↗

DOE OSTI2022

Characterization of nonlinear ultrasonic waves behavior while interacting with poor interlayer bonds in large-scale additive manufactured materials

Over the past decades, researchers have developed several nonlinear ultrasonic techniques for quality control of materials commonly used in different applications. Owing to the superior sensitivity of nonlinear ultrasound waves to small defects such as micro-cracks, their applicability in different nondestructive testing (NDT) problems has been investigated in numerous studies. These studies utilize frequency domain analysis to detect the generation of higher harmonics because of the formation of defects in the inspected medium. Frequency domain analysis based on the Fourier transform is a significant approach used in linear systems; however, it may not perform adequately on nonlinear systems. Hence, studies on nonlinear dynamics and physics consider analyzing systems' behavior in the phase-space domain. In contrast to the frequency domain analysis, which can result in information loss, analysis in the phase-space domain retains all the information regarding a system's states. Here, we investigate the nonlinearities induced by poor interlayer bonding in polymer-based additive manufactured parts in the phase-space domain. It is convenient to characterize the nonlinearity in the phase-space domain because it provides a geometrical representation of a system's states. Two types of low quality interlayer bond are considered. The first type is simulated artificially while the second type is manufactured by reducing the bond quality during the printing process. The analysis verified that the received ultrasonic signals exhibit classical nonlinear behavior in the phase-space domain while interacting with simulated poor interlayer bonds. In addition, the results showed that the behavior of ultrasonic waves is amplitude-dependent and evolves into models that have not been previously reported. Furthermore, Largest Lyapunov Exponent (LLE) is used to quantify the behavior of nonlinear ultrasonic waves while interacting with poor interlayer bonds. Using LLE, it was observed that the divergence rate of the phase-space trajectories depends on the amplitude of the excitation. This observation quantitatively proves that nonlinear behavior of ultrasound while interacting with poor interlayer bonds can be amplitude-dependent. The results of both simulated and inherent poor interlayer bond cases showed that LLE can be used as a reliable quantitative damage-sensitive feature to detect and potentially characterize weak bonds, which are difficult to detect using conventional approaches. Additionally, the reported results in the phase-space domain provide a basis for proposing a new mathematical model for ultrasonic waves interacting with poor interlayer bonds.

36 MATERIALS SCIENCE↗