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Emerging hierarchical dislocation structures: Insights from scanning electron microscopy-electron backscatter diffraction in situ tensile testing and multifractal analysis

Understanding the evolution of dislocation structures during plastic deformation is critical for predicting the mechanical performance of metallic materials. In this work, we applied in situ scanning electron microscopy/electron backscatter diffraction tensile testing combined with multifractal (MF) analysis to assess deformation-induced dislocation structure evolution in solution-annealed 304 L stainless steel, both in its as-received and neutron-irradiated states (5.4 displacements per atom). The analysis of kernel average misorientation patterns revealed the formation of hierarchical dislocation arrangements that exhibit clear MF scaling behavior. Despite pronounced visual differences between nonirradiated and irradiated specimens—most notably, the appearance of dislocation channels after irradiation—the singularity spectra suggest that both conditions give rise to similar underlying hierarchical structures. MF analysis provides a quantitative measure of the spatial complexity and self-organization of dislocation patterns, highlighting the accelerated emergence and evolution of the dislocation structures in irradiated polycrystalline materials, as well as the limitation of their spatial extent. The findings indicate that irradiation not only modifies microstructure but also alters correlation-driven dislocation organization. More generally, they demonstrate that MF analysis is a powerful tool for probing mesoscale deformation mechanisms.

Dislocation structures

A Procedure to Quantify Interlaminar Damage in Refractory Composites by In-Situ Micro-X-Ray Computed Tomography

Refractory composites are relevant for hot-structure applications on re-entry vehicles. To develop optimized high-performance hot structures, accurate material property data is required. Material properties that often limit design in two-dimensional (2-D) composites are interlaminar strengths. A better understanding of the failure mechanisms for interlaminar shear (ILS), interlaminar tension (ILT), and curved-beam interlaminar tension (CB-ILT) tests can provide insight on improving the design and fabrication of refractory composites. In-situ tests were performed to capture the progressive failure in American Society for Testing and Materials (ASTM) sized ILS (ASTM D3846), ILT (ASTM D7291), and CB-ILT (ASTM D6415) specimens. Before measuring internal damage of refractory composites specimens, the methodology of the test setup warrants a complete and thorough discussion. Detail on the test procedure, test stand design, micro-x-ray computed tomography (CT) configuration, data processing, and CT system uncertainty is discussed. Through keeping the many parameters of the CT system consistent, the uncertainty of the CT system was minimized, optimizing the quality of measurements. The overall quality of a CT scan can be quantified by three metrics: voxel resolution, minimal voxel resolution feature detection, and directional variability. A better understanding of the progressive failure mechanisms of refractory composites is provided by the results of both the present discussion and the one found in the accompanying paper titled “Analysis of Interlaminar Damage in Refractory Composites by In-Situ Micro-X-Ray Computed Tomography”.

In-situ micro-x-ray CT

Analysis of Interlaminar Damage in Refractory Composites by In-Situ Micro-X-Ray Computed Tomography

Refractory composites are relevant for hot-structure applications on re-entry vehicles. To develop optimized high-performance hot structures, accurate material property data is required. Material properties that often limit design in two-dimensional (2-D) composites are interlaminar strengths. A better understanding of the failure mechanisms for interlaminar shear (ILS), interlaminar tension (ILT), and curved-beam interlaminar tension (CB-ILT) tests can provide insight on improving the design and fabrication of refractory composites. In-situ tests were performed to capture the progressive failure in American Society for Testing and Materials (ASTM) sized ILS (ASTM D3846), ILT (ASTM D7291), and CB-ILT (ASTM D6415) specimens. The present study investigates the change in material behavior by examining the macro porosity change in in-situ ILS tests, the mesoscale and inter-ply porosity changes in flatwise in-situ ILT tests and the change in per-ply delamination in in-situ CB-ILT tests.

In-situ Damage Characterization

Intricacies of Using Kevlar Cord and Thermal Knives in a Deployable Release System: Issues and Solutions

The utilization of Kevlar cord and thermal knives in a deployable release system produces a number of issues that must be addressed in the design of the system. This paper proposes design considerations that minimize the major issues, thermal knife failure, Kevlar cord relaxation, and the measurement of the cord tension. Design practices can minimize the potential for thermal knife laminate and element damage that result in failure of the knife. A process for in-situ inspection of the knife with resistance, rather than continuity, checks and 10x zoom optical imaging can detect damaged knives. Tests allow the characterization of the behavior of the particular Kevlar cord in use and the development of specific prestretching techniques and initial tension values needed to meet requirements. A new method can accurately measure the tension of the Kevlar cord using a guitar tuner, because more conventional methods do not apply to arimid cords such as Kevlar.

Stewart, Alphonso

Intricacies of Using Kevlar and Thermal Knives in a Deployable Release System: Issues and Solutions

The utilization of Kevlar cord and thermal knives in a deployable release system produces a number of issues that must be addressed in the design of the system. This paper proposes design considerations that minimize the major issues, thermal knife failure, Kevlar cord relaxation, and the measurement of the cord tension. Design practices can minimize the potential for thermal knife laminate and element damage that result in failure of the knife. A process for in-situ inspection of the knife with resistance, rather than continuity, checks and 10x zoom optical imaging can detect damaged knives. Tests allow the characterization of the behavior of the particular Kevlar cord in use and the development of specific pre-stretching techniques and initial tension values needed to meet requirements. A new method can accurately measure the tension of the Kevlar cord using a guitar tuner, because more conventional methods do not apply to arimid cords such as Kevlar.

Stewart, Alphonso C.

Evaluation of thermal and mechanical loading effects on the structural behavior of a SiC/titanium composite

Composite specimens of titanium-15-3 matrix reinforced with continuous SCS-6 silicon carbide fibers were tested under a variety of thermal and mechanical loadings. A combined experimental/finite element approach was used to estimate the effective in-situ modulus of the matrix material and to evaluate changes in modulus due to the applied loads. Several fiber orientations were tested. Results indicate that the effect of the thermal loads on composite stiffness varies with fiber orientation. Applications of this method to test specimens damaged by uniaxial tension, thermal cycling, and isothermal fatigue loadings are used to illustrate that by monitoring overall structural behavior, changes in stiffness caused by thermomechanical loading can be detected.

Grady, Joseph E.

Mechanical properties of lunar regolith and lunar soil simulant

Through the Surveyor 3 and 7, and Apollo 11-17 missions a knowledge of the mechanical properties of Lunar regolith were gained. These properties, including material cohesion, friction, in-situ density, grain-size distribution and shape, and porosity, were determined by indirect means of trenching, penetration, and vane shear testing. Several of these properties were shown to be significantly different from those of terrestrial soils, such as an interlocking cohesion and tensile strength formed in the absence of moisture and particle cementation. To characterize the strength and deformation properties of Lunar regolith experiments have been conducted on a lunar soil simulant at various initial densities, fabric arrangements, and composition. These experiments included conventional triaxial compression and extension, direct tension, and combined tension-shear. Experiments have been conducted at low levels of effective confining stress. External conditions such as membrane induced confining stresses, end platten friction and material self weight have been shown to have a dramatic effect on the strength properties at low levels of confining stress. The solution has been to treat these external conditions and the specimen as a full-fledged boundary value problem rather than the idealized elemental cube of mechanics. Centrifuge modeling allows for the study of Lunar soil-structure interaction problems. In recent years centrifuge modeling has become an important tool for modeling processes that are dominated by gravity and for verifying analysis procedures and studying deformation and failure modes. Centrifuge modeling is well established for terrestrial enginering and applies equally as well to Lunar engineering. A brief review of the experiments is presented in graphic and outline form.

Steven W Perkins

Tethered Dynamics Explorer and Tethered Atmospheric Probe - A low-cost, low-risk tethered satellite program

A tethered satellite flight program to test theoretical studies of tether concepts is proposed. The program consists of multiple flights of an ELV such as the Delta II, using the Small Expendable Deployment System (SEDS) to deploy two instrumented satellite payloads, the Tethered Dynamics Explorer (TDE) and the Tethered Atmospheric Probe (TAP). The applications and characteristics of the TDE and the TAP are described, including verification of the SEDS, the validation of the dynamics and control model for low-tension deployment and the force and moment instrumentation, the demonstration of tether initiated reentry, the collection of in-situ atmospheric and aerothermodynamic data, and the study of long-term tether exposure.

Deloach, R.

In-Situ Pressure Measurements During the Detached Growth of Germanium

Crystal growth by the vertical Bridgman method in which there is little or no contact between the wall and the crystal has been termed detached solidification. Detachment has been observed frequently in previous microgravity experiments, and has been reported under some terrestrial conditions as well. It is expected that detachment can be conditioned by establishing an appropriate pressure difference below and above the melt. To test this hypothesis, an experimental technique has been developed to measure this pressure difference during the growth of germanium by the vertical Bridgman method. The apparatus allows for both monitoring the pressures and actively controlling them during growth. For a given melt height, there is a maximum pressure difference attainable before gas bubbles up through the melt. This maximum pressure increases with increasing melt height. As the melt height approaches zero, the maximum pressure difference, about 20 mbar in these experiments, is determined by the surface tension and gap width of the meniscus at the bottom of the melt.

Volz, M. P.

Reducing Extra-Terrestrial Excavation Forces with Percussion

High launch costs and mission requirements drive the need for low mass excavators with mobility platforms, which in turn have little traction and excavation reaction capacity in low gravity environments. This presents the need for precursor and long term future missions with low mass robotic mining technology to perform In-Situ Resource Utilization (ISRU) tasks. This paper discusses a series of experiments that investigate the effectiveness of a percussive digging device to reduce excavation loads and thereby the mass of the excavator itself. The goal of percussive excavation is to fluidize dry regolith in front of the leading edge of the tool by mechanically separating the microscopic interlocking grains resulting in a reduced force needed to shear the soil. There are several variables involved with this technique; this experiment varied: Impact energy, frequency, and excavation speed and held constant: impact direction, depth of cut, angle of tool, and soil bulk density. The test apparatus consisted of an aluminum truss bridge with a central pivoting arm. Attached to the arm was a winch with a load cell in line that recorded the tension in the cable and therefore the excavation load. The arm could be adjusted for excavation depth which was recorded along with the arm angle relative to the bridge. A percussive mechanism and 30" wide pivoting bucket were attached at the end of the arm simulating a basic backhoe with a percussion direction tangent to the direction of . movement. Internally the mechanism used a set of die springs and barrel cam to produce the percussive blow. By changing the springs and the speed of the motor the impact energy and frequency of percussion could be varied independently. Impact energies from 11.2J to 30.5J and frequencies from 0 BPM to 700 BPM were investigated. A reduction in excavation force of as much as 51% was achieved in this experimental investigation. Smaller percussive digging implements, tested by others, have achieved a reduction of as much as 72%. This paper will examine the effects of impact energy, frequency, scaling and their effect on excavation forces in a dry granular material such as lunar regolith. The past several years have shown an increasing interest in mining space resources both for exploration and commercial enterprises. This work studied the benefits and risks of percussive excavation and prelimin~ry results indicate that this technique may become an enabling technology for extra-terrestrial excavation of regolith and ice.

Schuler, Jason

In-Situ Scanning Electron Microscope Experiments for Microscale Mechanical Testing and Validated Modeling of Fiber Reinforced Thermoplastics

A novel, in-situ, scanning electron microscope (SEM) mechanical testing capability for materials at the microscale which provides experimental validation to a machine learning (ML) toolset for full-field validation of physics-based micromechanics models is being developed by researchers at NASA Glenn Research Center. These are enabling technologies for the integration of multiscale digital twins for materials into system level models which will result in the improved performance, material discovery, reduced production cost and time, rapid characterization, and prognostic structural health monitoring (SHM) for materials and structures for extreme environments in support of NASA space exploration missions. In order to bridge the material structure-to-system gap for digital twins, physics-based models must be experimentally validated at multiple length scales. Seminal microscale experiments, conducted at the Air Force Research Laboratory (AFRL), were limited to transverse compression of single-layer, unidirectional thermoset polymer matrix composite (PMC) micropillar specimens [1]. The early phases of the current project followed those initial results and setup to reproduce the compression testing of PMC material on the custom-built piezoelectric actuated micromechanical testing rig built by MicroTesting Solutions LLC. In this work, samples of thermoplastic PMC material were first machined into 3 mm cubes, and then further machining and final milling was done using a Focused Ion Beam (FIB). The initial experiment was done on a pillar roughly 20 µm x 20 µm x 40 µm tall. Additional pillars were milled with final sizes ranging from 20 µm x 20 µm x 40 µm tall to 40 µm x 40 µm x 65 µm tall. A speckle pattern for in-situ full-field measurements using Digital Image Correlation (DIC) was applied with platinum, which was coated on the surface, and then the FIB was used to mill away some of the coating to produce an irregular pattern of Pt on the pillar surface. The samples were loaded into the custom testing rig and placed into the SEM and loaded under compression until failure. Images were collected in the SEM during testing. Post-processing of the images was conducted using DIC to obtain full-field displacement and strain measurements elucidating the role of the matrix as well as fiber-fiber interaction at the microscale within the composite subjected to compression loading well into the non-linear regime of the material. Moreover, the evolution of fiber-matrix debonding and matrix cracking is observed in-situ at the microscale. This data, along with images segmented with a newly developed ML toolset [2], was used to create and validate physics-based micromechanics models. An image of the failed micropillar is shown in Figure 1. The techniques developed in the initial compression experiment was tailored to the validation needs of the models and expanded to include different sized samples as well as possibly tension and fatigue.

Laura Wilson

Real time acousto-ultrasonic NDE technique for monitoring damage in ceramic composites under dynamic loads

Research effort was directed towards developing a near real-time, acousto-ultrasonic (AU), nondestructive evaluation (NDE) tool to study the failure mechanisms of ceramic composites. Progression of damage is monitored in real-time by observing the changes in the received AU signal during the actual test. During the real-time AU test, the AU signals are generated and received by the AU transducers attached to the specimen while it is being subjected to increasing quasi-static loads or cyclic loads (10 Hz, R = 1.0). The received AU signals for 64 successive pulses were gated in the time domain (T = 40.96 micro sec) and then averaged every second over ten load cycles and stored in a computer file during fatigue tests. These averaged gated signals are representative of the damage state of the specimen at that point of its fatigue life. This is also the first major attempt in the development and application of real-time AU for continuously monitoring damage accumulation during fatigue without interrupting the test. The present work has verified the capability of the AU technique to assess the damage state in silicon carbide/calcium aluminosilicate (SiC/CAS) and silicon carbide/ magnesium aluminosilicate (SiC/MAS) ceramic composites. Continuous monitoring of damage initiation and progression under quasi-static ramp loading in tension to failure of unidirectional and cross-ply SiC/CAS and quasi-isotropic SiC/MAS ceramic composite specimens at room temperature was accomplished using near real-time AU parameters. The AU technique was shown to be able to detect the stress levels for the onset and saturation of matrix cracks, respectively. The critical cracking stress level is used as a design stress for brittle matrix composites operating at elevated temperatures. The AU technique has found that the critical cracking stress level is 10-15% below the level presently obtained for design purposes from analytical models. An acousto-ultrasonic stress-strain response (AUSSR) model for unidirectional and cross-ply ceramic composites was formulated. The AUSSR model predicts the strain response to increasing stress levels using real-time AU data and classical laminated plate theory. The Weibull parameters of the AUSSR model are used to calculate the design stress for thermo-structural applications. Real-time AU together with the AUSSR model was used to study the failure mechanisms of SiC/CAS ceramic composites under static and fatigue loading. An S-N curve was generated for a cross-ply SiC/CAS ceramic composite material. The AU results are corroborated and complemented by other NDE techniques, namely, in-situ optical microscope video recordings and edge replication.

Tiwari, Anil