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Materials Characterization, Prediction, and Control Project: Summary Report on Material Characterization, Part 4

The Pacific Northwest National Laboratory (PNNL) undertook the Materials Characterization, Prediction, and Control (MCPC) Laboratory Directed Research and Development Project to advance understanding of nuclear material processing and enable multifold acceleration in the development and qualification of new material systems in national security and advanced energy applications (Smith 2021). The MCPC Project executed research across three scientific vertices—material characterization, predictive modeling, and data analytics—with extensive support by a data curation and management team. The central technical objective in the MCPC Project was to improve the prediction and characterization of the process-structure-property relationships within the microstructurally refined region of stainless-steel samples prepared utilizing friction stir processing (FSP). Application of the FSP technique is well established at PNNL within the Solid Phase Processing capability through many years of investment across a range of materials and applications (PNNL 2024).

36 MATERIALS SCIENCE↗

Solid Phase Gradient Alloying Method via ShAPE

Alloying has been used to confer desirable properties to various metallic systems since the bronze age. For example, Ni, Mn, and Cr are alloyed into an Fe matrix to make steel, which has improved strength and corrosion resistance (as displayed in Fig. 1). In addition to the type of alloying elements, the amount of alloying elements added into a matrix is also very critical for a material’s mechanical property, physical property, machinability, and cost. Conventionally, new alloys are discovered by combining alloy precursors and elemental constituents into a mixture and melting them together. The solidified product or ingot represents a usually non-homogeneous combination of the chemistry with a microstructure dictated by the physics of solidification. It is time and energy intensive to optimize the alloying amounts via the casting process and hence, economically not conducive to rapid alloy discovery. In addition, the cast microstructure seen in the as-cast ingot is often not the ideal, nor even desired structure for optimized performance. Cast materials often need further processing such as homogenization, annealing, and deformation work put in through rolling, forging, extruding, etc. to have favorable microstructures and properties. A faster method to discover new alloy combinations and evaluate them in their worked or processed form is needed. Recently, Laser Engineered Net Shaping was applied to fabricate gradient compositional material for alloy designing. However, the mechanical properties of this gradient alloy were poor due to the existence of impurities, oxidation and cracks that are inherent in the melt-solidification process. Because of these limitations, we propose to use a solid-phase process (ShAPE) to create bulk materials (extrudates) that vary in composition from one end of the extruded solid to the other. Various manufacturing methods for alloy design including conventional casting method, laser based combinatorial method and current solid phase gradient alloying method are displayed and compared in Fig. 2. ShAPE machine and a schematic of ShAPE process are displayed in Fig. 3. Starting material is processed by a rotating and plunging die to form an extrudate. We are proposing through this methodology to invent a new, bulk-scale combinatorial technique. With this novel technique, alloying element can be dissolved into the matrix with a continued gradient without bulk melting. Formation of inter-metallics and defects originating from melt processing can be avoided. In addition, the ShAPE process creates the mixed alloy chemistry, and meanwhile subjects the material to severe plastic strain, which induces the favorable “worked” microstructure. Products from the ShAPE process can be tested in hardness directly providing a path to rapid evaluation of mechanical properties. The ability to create graded structures using friction stir processing (FSP) has been demonstrated, however using the ShAPE process we believe will lead to much faster and higher fidelity results. When combined with high throughput screening methods of physical, mechanical and microstructural property characterization, efficiency and accuracy of alloy design can be significantly improved.

36 MATERIALS SCIENCE↗

Materials Characterization, Prediction, and Control Project: Characterization of 316L Stainless Steel after Solid Phase Processing using Ultrasonic NDE Method

The Pacific Northwest National Laboratory undertook the Materials Characterization, Prediction, and Control Laboratory Directed Research and Development Project to advance understanding of nuclear material processing and enable multifold acceleration in the development and qualification of new material systems produced via advanced manufacturing methods, such as solid phase processing, for use in national security and advanced energy applications (Smith 2021). A motivation of the Materials Characterization, Prediction, and Control Project was to demonstrate ultrasonic testing as a nondestructive evaluation method to complement traditional destructive methods for characterizing material microstructure with emphasis on grain size determination using a method that may have future applications for real-time inline process monitoring. The objective of the work described in this report is to establish the process and an analysis method for measuring grain sizes of polycrystalline metals with ultrafine grains using ultrasonic shear wave backscattering, building on prior studies on coarser-grained material. The work involves five tasks: Measured ultrasonic backscattering experimentally for a series of 316L stainless steel specimens with various grain sizes made by friction stir processing. Calculated ultrasonic backscattering coefficients from experimental data based on a physical measurement model. Measured ground truth grain sizes of the specimens from electron backscatter diffraction grain boundary images using a generalization of the ASTM E112 (ASTM 2021) intercept method. Built a curve of ultrasonic backscattering coefficients versus the ground truth intercept-based grain sizes to determine the correlation between mean grain sizes and ultrasonic measurements. Demonstrated the ability of using the correlation curve to deduce grain sizes with measured ultrasonic backscattering coefficients for a few 316L stainless steel specimens whose grain sizes were unknown beforehand but were targeted to be an extrapolation to larger grain sizes than used to formulate the correlation curves. Experimental procedures and computational algorithms are developed and validated for these tasks. This work establishes an ultrasonic technique for characterizing material microstructure with ultrafine grains that are often resulted by solid-phase processing. The technique is nondestructive, and it has the potential to be used for real time inline process monitoring. This work successfully demonstrates the viability of an ultrasonic nondestructive evaluation method for microstructural characterization of material having ultrafine grain structure (as small as 1?mm) and produced by an advanced manufacturing method. This includes a demonstration of the method to extrapolate to other conditions. While not demonstrated here, the method is expected to be viable for in-line, or near-inline, process monitoring in advanced manufacturing applications with suitable consideration for access of instrumentation to the material being manufactured.

316 L Stainless Steel↗

Additive manufacturing of metal matrix composites

Although Metal matrix composites (MMCs) are superior to most sought-after metallic alloys, their challenging fabricability has limited their widespread use in bulk-form applications. Among the many advanced fabrication techniques, Additive Manufacturing (AM), owing to its unique capabilities to produce near-net shapes, has drawn significant traction in the past two decades, especially for materials that are difficult to process using traditional methods. However, unlike pure metal/alloy systems, MMCs are highly sensitive to the processing conditions prevailing in AM techniques due to factors such as the high melting point of reinforcement particles and the potential for in-situ reactions. Therefore, it may be a while before metal matrix composites are commercially produced via AM. This review will discuss the current state-of-the-art design, fabricability, and performance of various additively manufactured MMCs. A particular focus will be on microstructural evolution and microstructure-property relationships. The most employed AM techniques, such as directed energy deposition, powder bed fusion, binder jetting, sheet lamination, and solid-state friction stir processing, are fundamentally different in terms of thermo-kinetics, forming the perspective for this review. A detailed comparison of microstructural evolution and process parameter optimization, including feedstock preparation methods and the role of machine learning and modeling among the different AM processes, is also presented. Finally, a critical evaluation of emerging AM technologies for MMCs is also provided, highlighting their potential advantages and challenges.

36 - MATERIALS SCIENCE↗

Effect of temperature on the fatigue cracking mechanisms in A356 Al alloy

This work builds on our previous investigation of the room temperature fatigue cracking mechanisms of an A356 Al alloy. Here, we analyze the elevated temperature fatigue cracking mechanisms in cast and friction stir processed (FSP) A356, and contrast them with the room temperature behavior. Two sets of FSP parameters were used to modify the microstructure of the cast alloy. After heat treatment, both the FSPed microstructures exhibited severe abnormal grain growth (AGG) leading to a very wide grain size distribution (from a few microns to a few millimeters). During room temperature fatigue tests, the FSP conditions exhibited significant improvements in fatigue lives, even up to an order of magnitude. However, with increasing temperature, the difference in the performance of the FSPed and Cast microstructures decreased until, at 200 °C, all three microstructural conditions exhibited similar fatigue response. Detailed electron back scattered diffraction (EBSD) imaging of failed fatigue specimens was used to study crack behavior. At room temperature, cracks initiated at defect sites or along persistent slip bands (PSBs) and propagated transgranularly. The grain boundaries acted as barriers to crack growth. At elevated temperatures, there was a complete role reversal of the grain boundaries. Cracks initiated along grain boundaries and propagated intergranularly in all microstructures. Below, we explore this transition of the cracking mechanism in detail.

Nelaturu, Plalgun↗

Generalizable Image Segmentation for Microstructure Characterization Through Integrated SEM and EBSD Analysis

We demonstrate generalizable semantic segmentation using minimal ground truth data. Correlated scanning electron microscopy (SEM) images and electron backscatter diffraction (EBSD) measurements of frictionstir processed 316L stainless steel plates were used to train deep learning models for grain boundary segmentation. Secondary electron (SE) imaging taken at an accelerating voltage of 10 keV correlated to EBSD-derived grain boundaries produced the best performing model. Notably, an ensemble of three models trained on a single SE image produced accurate segmentation over a series of BSE images of samples manufactured under different processing parameters, with a resultant mean absolute error in grain size of 0.34 µm. The striking generalizability of the models likely results from the similar escape depths of the SE training input and the EBSD training output and the reduced probability of dislocation artifacts appearing in the image. This finding highlights the importance of considering the physical principles behind imaging in the development of robust segmentation models for microstructure characterization.

Taufique, Mohammad Fuad Nur↗

Laser Ablation Cleaning of Self-Reacting Friction Stir Weld Seam Surfaces: A Preliminary Evaluation

Anodized aluminum panels were cleaned by three lasers at three separate sites with a view to determining whether more economical laser cleaning might supplant current manual cleaning methods for preparation of surfaces to be welded by the self-reacting friction stir process. Uncleaned panels yielded welds exhibiting residual oxide defect (ROD) and failing at very low stresses along the trace of the weld seam. Manually cleaned panels yielded welds without ROD; these welds failed at nominal stress levels along an angled fracture surface not following the weld seam trace. Laser cleaned panels yielded welds failing at intermediate stress levels. The inadequacy of the laser cleaning processes leaves questions: Was the anodized aluminum test too stringent to represent actual cleaning requirements? Were the wrong laser cleaning techniques/parameters used for the study? Is the laser cleaning mechanism inadequate for effective preweld surface cleaning?

Nunes, A. C., Jr.↗

Process Model for Friction Stir Welding

Friction stir welding (FSW) is a relatively new process being applied for joining of metal alloys. The process was initially developed by The Welding Institute (TWI) in Cambridge, UK. The FSW process is being investigated at NASA/MSEC as a repair/initial weld procedure for fabrication of the super-light-weight aluminum-lithium shuttle external tank. The FSW investigations at MSFC were conducted on a horizontal mill to produce butt welds of flat plate material. The weldment plates are butted together and fixed to a backing plate on the mill bed. A pin tool is placed into the tool holder of the mill spindle and rotated at approximately 400 rpm. The pin tool is then plunged into the plates such that the center of the probe lies at, one end of the line of contact, between the plates and the shoulder of the pin tool penetrates the top surface of the weldment. The weld is produced by traversing the tool along the line of contact between the plates. A lead angle allows the leading edge of the shoulder to remain above the top surface of the plate. The work presented here is the first attempt at modeling a complex phenomenon. The mechanical aspects of conducting the weld process are easily defined and the process itself is controlled by relatively few input parameters. However, in the region of the weld, plasticizing and forging of the parent material occurs. These are difficult processes to model. The model presented here addresses only variations in the radial dimension outward from the pin tool axis. Examinations of the grain structure of the weld reveal that a considerable amount of material deformation also occurs in the direction parallel to the pin tool axis of rotation, through the material thickness. In addition, measurements of the axial load on the pin tool demonstrate that the forging affect of the pin tool shoulder is an important process phenomenon. Therefore, the model needs to be expanded to account for the deformations through the material thickness and the forging affect of the shoulder. The energy balance at the boundary of the plastic region with the environment required that energy flow away from the boundary in both radial directions. One resolution to this problem may be to introduce a time dependency into the process model, allowing the energy flow to oscillate across this boundary. Finally, experimental measurements are needed to verify the concepts used here and to aid in improving the model.

Adams, Glynn↗

MCPC Friction Stir Welding (FSW) Process Data

Processing parameters and machine log data for the MCPC LDRD Agile investment is collected material samples processed. This dataset captures the selected processing parameters, machine logs captured during material processing, and descriptions of how characterization samples were extracted from processed plates of material. The collect characterization data is captured in other datasets.

316 Stainless Steel↗

Process Robustness of Friction Stir Dovetailing of AA7099 to Steel with In Situ AA6061 Interlayer Linking

Rolled homogeneous armor (RHA) steel was joined to aluminum alloy AA7099-T7451 with an interlayer of AA6061-T651 by single-pass friction stir dovetailing (FSD). The evolution of the AA7099/AA6061 and AA6061/steel interfacial microstructures and mechanical properties of the joints were examined. The AA6061 interlayer prevented Zn migration from the AA7099 to the steel during FSD and inhibited formation of brittle, Zn-rich, Fe-Al intermetallic compounds within the joint. The flow of the dissimilar aluminum alloys at the interface was controlled with a partially threaded friction stir welding pin and a dovetail geometric configuration optimized in previous work. The process robustness was explored to establish parameter windows by elucidating parametric effects on the relationship between process conditions and the joint’s microstructure and mechanical properties. Ranges of process forge force (50–70 kN) and interface temperature (475°C–515°C) consistently yielded joints with adequate performance. The load-carrying capacity in lap shear tensile tests was 2025 ? 100 N/mm.

Friction Stir Dovetailing, FSW, AA7099, AA6061, Ro↗

SLI Complex Curvature Friction Stir Weld Risk Reduction Program

The Space Launch Initiative Program (SLI) in conjunction with the National Center for Advanced Manufacturing (NCAM) will demonstrate the ability to produce large-scale complex curvature hardware using the self-reacting friction stir welding process. This multi-phased risk reduction program includes friction stir welding process development and manufacture of a 22-ft diameter quarter dome using a conventional tooling approach; it culminates in a 27.5-ft diameter quarter dome demonstration performed on a 5-axis Universal Weld System. The design, fabrication, and installation of the Universal Weld System is made possible through a collaboration between the State of Louisiana, NASA, and the University of New Orleans. The Universal Weld System, manufactured by MTS Systems Corporation, will be installed at the Michoud Assembly Facility in New Orleans, Louisiana, and will be capable of manufacturing domes up to 30 ft in diameter. All welding will be accomplished using the Adaptable Adjustable Pin Tool (AdAPT) weld head and controller manufactured by MTS. Weld parameters will be developed for an aluminum alloy in gauges ranging from 0.320 to 0.400 in. thick. Weld quality will be verified through radiography, mechanical property testing at ambient and LN2 temperatures, and metallurgical analysis. The AdAPT weld head will then be mounted on a 22-ft diameter dome tool, which will be modified to include a welding track and drive system for moving the AdAPT weld head along the weld joint. This tool will then be used to manufacture a 22-ft diameter dome of an aluminum alloy, with 0.320-in. constant thickness joints, consisting of three individual gore panels. Finally, the 27.5-ft diameter quarter dome will be welded on the Universal Weld System. The quarter dome will consist of three individual gore panels with weld lands tapering from 0.320 to 0.360 in. in thickness. With the demonstration of these welds, the ability to manufacture large diameter domes using the friction stir weld process in conjunction with a universal weld system provides a low risk approach to the fabrication of aluminum tanks for future launch vehicle applications.

Hartley, Paula J.↗

Friction Stir Welding Development

The research of this summer was a continuation of work started during the previous summer faculty fellowship period. The Friction Stir Welding process (FSW) patented by The Welding Institute (TWI), in Great Britain, has become a popular topic at the Marshall Space Flight Center over the past year. Last year it was considered a novel approach to welding but few people took it very seriously as a near term solution. However, due to continued problems with cracks in the new aluminum-lithium space shuttle external tank (ET), the friction stir process is being mobilized at full speed in an effort to mature this process for the potential manufacture of flight hardware. It is now the goal of NASA and Lockheed-Martin Corporation (LMC) to demonstrate a full-scale friction stir welding system capable of welding ET size barrel sections. The objectives this summer were: (1) Implementation and validation of the rotating dynamometer on the MSFC FSW system; (2) Collection of data for FSW process modeling efforts; (3) Specification development for FSW implementation on the vertical weld tool; (4) Controls and user interface development for the adjustable pin tool; and (5) Development of an instrumentation system for the planishing process. The projects started this summer will lead to a full scale friction stir welding system that is expected to produce a friction stir welded shuttle external tank type barrel section. The success of this could lead to the implementation of the friction stir process for manufacturing future shuttle external tanks.

Romine, Peter L.↗

Unraveling the Processing Parameters in Friction Stir Welding

In friction stir welding (FSW), a rotating threaded pin tool is translated along a weld seam, literally stirring the edges of the seam together. To determine optimal processing parameters for producing a defect free weld, a better understanding of the resulting metal deformation flow path or paths is required. In this study, various markers are used to trace the flow paths of the metal. X-ray radiographs record the segmentation and position of the wire. Several variations in the trajectories can be differentiated within the weld zone.

Schneider, Judy↗

Investigation of Friction Stir Welding of Al Metal Matrix Composite Materials

The innovative process of Friction Stir Welding (FSW) has generated tremendous interest since its inception about a decade or so ago since the first patent in 1991 by TWI of Cambridge, England. This interest has been seen in many recent international conferences and publications on the subject and relevant published literature. Still the process needs both intensive basic study of deformation mechanisms during this FSW process and analysis and feasibility study to evaluate production methods that will yield high quality strong welds from the stirring action of the appropriate pin tool into the weld plate materials. Development of production processes is a complex task that involves effects of material thickness, materials weldability, pin tool design, pin height, and pin shoulder diameter and related control conditions. The frictional heating with rotational speeds of the pin tool as it plunges into the material and the ensuing plastic flow arising during the traverse of the welding faying surfaces provide the known special advantages of the FSW process in the area of this new advanced joining technology.

Diwan, Ravinder M.↗

Friction Stir Welding of Steel Alloys

The friction stir welding process has been developed primarily for the welding of aluminum alloys. Other higher melting allows such, as steels are much more difficult to join. Special attention must be given to pin tool material selection and welding techniques. This paper addresses the joining of steels and other high melting point materials using the friction stir welding process. Pin tool material and welding parameters will be presented. Mechanical properties of weldments will also be presented. Significance: There are many applications for the friction stir welding process other than low melting aluminum alloys. The FSW process can be expanded for use with high melting alloys in the pressure vessel, railroad and ship building industries.

Ding, R. Jeffrey↗

Ultrasonic Stir Welding

NASA Marshall Space Flight Center (MSFC) developed Ultrasonic Stir Welding (USW) to join large pieces of very high-strength metals such as titanium and Inconel. USW, a solid-state weld process, improves current thermal stir welding processes by adding high-power ultrasonic (HPU) energy at 20 kHz frequency. The addition of ultrasonic energy significantly reduces axial, frictional, and shear forces; increases travel rates; and reduces wear on the stir rod, which results in extended stir rod life. The USW process decouples the heating, stirring, and forging elements found in the friction stir welding process allowing for independent control of each process element and, ultimately, greater process control and repeatability. Because of the independent control of USW process elements, closed-loop temperature control can be integrated into the system so that a constant weld nugget temperature can be maintained during welding.

Nabors, Sammy↗

An innovative and alternative approach toward gear fabrication

In this paper, we present the first demonstration of single-step gear manufacturing via an innovative in-situ friction stir forging approach. This novel process is a natural extension to the friction stir processing technique and relies on shear and normal stresses to form the complex shapes. Friction stir welding pin tool with shoulder is plunged at high revolutions per minute (rpm) into the sample to heat it to the desired temperature and enable plastic flow. Then, the tool is forged at high plunge rate to form the desired structurally-sound and defect free complex shapes. To better visualize the process the experiments are complemented by a 3D thermomechanically coupled, smoothed particle hydrodynamics (SPH) model to understand the material flow pattern both radially and through thickness in the gear teeth, plastic strain distribution, and temperature profile. We have demonstrated application of I-FSF to inherently poor formable AZ31 Mg, AA 7075-T6, and AA5083–10 vol% TiB 2 composite and fabricated 14-tooth spur gears from these materials with minimal farther machining. In conclusion, microstructure of the forged gears exhibited a directional material flow pattern due to the normal forging action and refinement of grains to 6–13 μm through dynamically recrystallization across the radial, through-thickness direction, which is in good agreement with the corresponding SPH simulation results.

42 ENGINEERING↗

Gradient process parameter optimization in additive friction stir deposition of aluminum alloys

As one of the most novel additive manufacturing methods, currently selection and optimization of processing parameters in additive friction stir deposition (AFSD) have mainly relied on experiments and subsequent characterization of microstructural and mechanical properties. Such approaches are both time- and resource-consuming. Therefore, an ultrasound elastography enhanced gradient process parameter optimization method was applied in the present work to obtain a window of optimized processing parameters for AFSD processing of aluminum alloy by varying both rotational and linear deposition speeds. Further, the quality of AFSD processed layer was investigated for physical nature of surface, dynamic elastic modulus, and microstructural aspects in cross-sections of the deposited layer. The efficiency in exploring process parameters was significantly enhanced by implementing a high-throughput screening experimental design based on application of gradient process parameters and continuous ultrasound elastographs. In addition, the applied ultrasonic elastography technique assisted in evaluating the homogeneity in microstructure and mechanical properties of AFSD sample over the entire gradients of the process parameters. The techniques adopted in current work can be further extended to identify suitable parameters for AFSD fabrication of components with desired mechanical properties such as hardness, fatigue, etc.

36 MATERIALS SCIENCE↗