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Ashle M. PageNorth Carolina State University

Faculty Mentor: Wesley TayonNASA Langley Research Center

Quantifying Precipitate Size and Distribution in Aluminum Alloy

Friction Stir Welds for Aerospace Structures

ABSTRACTIn an effort to produce spacecraft and launch vehicles for missions outside of low Earth orbit and beyond, researchers have experimented with an innovative manufacturing process that combines friction stir welding (FSW) and spin-forming (SF). These techniques have been ap-plied in the manufacture of a single-piece crew module, like the Orion capsule, with alumi-num-lithium (Al-Li) alloy 2195 that exhibits low density and improved mechanical properties. However, abnormal grain growth (AGG) occurs within the FSW microstructure during solu-tion heat treatment (SHT), resulting in weakened mechanical properties. To suppress AGG, re-searchers have investigated heat treatments known as intermediate annealing treatments (IATs) prior to the SHT. Grains and their boundaries have been evaluated previously to determine the benefits of IATs. The purpose of this study was to develop a technique to examine the effective-ness of IATs by analyzing the role that precipitate particles have in the propagation of AGG. In order to evaluate the microstructure, images of the precipitate particles were captured us-ing a scanning electron microscope (SEM) equipped with a backscatter detector. Backscatter electron (BSE) images were analyzed to determine precipitate population, average size, and area fraction. Results for various IAT time and temperature combinations were compared in relation to effectiveness at mitigating AGG in order to develop more efficient manufacturing of aerospace structures.

0.4% silver, and 0.4% magnesium (weight %). Every 1 wt. % of Li increases the elas-tic modulus by 6% and reduces the density by 3% [11]. Alloy 2195 was incorporated in the final redesign of the space shuttle exter-nal tank, which became known as the Super Lightweight External Tank. The redesign of the tank and switch from conventional Al alloy 2219 to Al-Li alloy 2195 saved 7,500 pounds of weight [13]. NASA researchers are further investigating the use of alloy 2195 on future mission structures including the Orion Multi-Purpose Crew Vehicle [2].

Aluminum is used in many applications in the aerospace industry due to its low

density and resistance to corrosion. However, pure aluminum exhibits low tensile strength [14]. To increase the strength of its mechani-cal properties, alloying elements are added to aluminum. In this study, aluminum-lithium (Al-Li) alloy 2195 was the targeted mate-rial due to its combination of lower density and increased strength compared to conven-tional non-Li aluminum alloys. Composed of primarily aluminum, alloy 2195 contains only about 1% lithium with 4% copper,

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microstructure of the FSW. The large grains associated with AGG negatively impact the strength and ductility of the FSW region [12].

AGG has gained recent attention in alumi-num friction stir welds because of the detri-ment in mechanical properties. AGG is tied to microstructural instability in FSW that may arise from a variety of factors including

manufacturing cost compared to the current, multi-piece manufacturing method [2].

The FSW process mechanically stirs two materials together under a forging pressure to form high-strength welded joints. A rotating FSW tool is plunged into the material at the joint between the two plates. Through rapid heating and plastic deformation, the material

Current designs of launch vehicles and crew modules used in both manned travel and cargo transit into space involve multi-piece constructions that increase the amount of time and labor required for manufactur-ing. To simplify this process and reduce the manufacturing cost, researchers have ex-plored a new method that combines friction stir welding (FSW) with spin-forming (SF) in order to develop a single-piece structure [3, 14]. Commercial Al-Li plate sizes are not large enough to enable fabrication of a crew module from a single plate. Friction stir welding is used strictly to join two plates to provide an adequate sized spin-forming blank. The blank is spin-formed over a man-drel to form the desired shape as illustrated in Figure 1. Compared to the current multi-piece construction, the new approach elimi-nates 14 welds, thereby reducing the poten-tial for weld defects and decreasing the risk for catastrophic failure. Spin-forming is a near-net shape manufacturing technology as there is little material wasted during the pro-cess. This is considered a ‘greener’ manufac-turing technique and ultimately reduces the

is softened and joined together. Unlike con-ventional fusion welding, no melting occurs in the FSW process. Because it is solid-state process, FSW also eliminates many of the defects associated with fusion welding tech-niques such as shrinkage and solidification cracking [10].

The friction stir welded blank is spin-formed to shape at hot-forming temperatures by pressing the material over a shaped man-drel. After spin-forming, the material under-goes a solution heat treatment (SHT) and immediate water quench [4]. The SHT step creates a supersaturated solution that is ideal for subsequent nucleation of strengthening precipitates. Following SHT, the material is artificially aged to the T6 temper [8]. During this process, small precipitates nucleate and coarsen to further increase the strength of the material [15].

During the SHT step, abnormal grain growth (AGG) occurs within the FSW micro-structure [1]. AGG is characterized by rapid, preferential growth of individual grains that consume the recrystallized, fine-grained

Figure 1. Schematic of the spin-forming process (adapted from [2]).

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which is similar to the deformation that occurs during the spin-forming process. Material was hot rolled near the spin-forming temperature with a 25% thickness reduction to study the effect of thermal processing on the FSW microstructure and development of AGG. Researchers investigated heat treat-ments known as intermediate annealing treat-ments (IATs) prior to the SHT to stabilize the microstructure and promote continuous grain growth rather than AGG [3]. Previous work addressed the impact of the IAT on grain size, texture, and grain boundary distributions and found correlations between grain boundaries. Specifically, AGG occurred in regions with a greater density of low-angle grain boundar-ies, which are known to be less mobile than high angle boundaries [15, 2].

The objective of this study is to develop a methodology to characterize the distribution of precipitate particles and study the impact of IATs on those particles. These particles impact grain growth and may serve to pin the grain boundaries through a mechanism known as Zener drag [12, 2]. Hypothetically, the most effective pinning particles are small in size and have a uniform distribu-tion throughout the material. Through image analysis, precipitate microstructures within the FSW region were examined to determine the effect of precipitate population, size, and

In this study, several samples that were subjected to IATs at various degrees were evaluated. All of the samples were taken from the FSW region of a 2195 T3M4 plate with a starting thickness of approximately 1.6 inches that was reduced 25% through hot rolling. Tested samples were named accord-ing to processing periods. Specimens were then exposed to different IATs at various temperatures and times. The list of samples with their associated IAT combinations is displayed in Table 1.

In order to image the microstructure, sam-ples were mechanically polished for both op-tical metallography and electron microscopy. Using an automated polisher, the samples were mechanically polished with 600, 800, and 1200 grit silicon carbide (SiC) paper for 3 to 6 minutes per grit step. After completion of the coarser grinding stage, the samples were polished using a 0.05 µm colloidal sil-ica suspension on a felt-like polishing cloth.

Each sample was imaged in a scanning electron microscope (SEM) at the quarter-thickness, or t/4, location shown in through-thickness optical micrographs for each sample in Figure 2. This area was chosen because it exhibited the greatest net effect of the IAT on suppressing AGG. Each sample was photo-graphed at 5 various sites at the t/4 location to provide a sufficient statistical representation

heterogeneous distributions of crystallo-graphic texture, grain boundary mobility and energy, grain size, and precipitate particles [5].

NASA researchers have performed labo-ratory studies to simulate the effect of spin-forming deformation on the FSW material. Deformation introduced by hot rolling re-duces the plate thickness via compression,

area fraction on the extent of AGG following the SHT. The precipitate particles were char-acterized before and after the IAT in order to analyze the role of IATs in limiting AGG to improve the manufacturing of aerospace structures.

Experimental Procedures

Ashle M. Page

Table 1. Sample designations with corresponding IAT time-temperature combinations.

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of each area using backscatter electron (BSE) imaging. At 1000x, the SEM revealed many aspects of the microstructure that were not visible in the optical images. The BSE detec-tor collected electrons scattered as a function of sample composition. Due to atomic num-ber contrast, the copper (Cu) rich precipitates were highlighted against the Al matrix and easily identified in BSE imaging. The BSE images were then analyzed using ImageJ (Image Processing and Analysis in Java) soft-ware [13]. Brightness and contrast thresholds were adjusted to better separate the precipi-tates from the surrounding grain structure. The SEM scale bar on the image was used to calibrate the number of pixels per microm-eter to accurately measure particle size. The software then measured the number of par-ticles (count), average particle size (average size), and area fraction of particles (% area) for each image. Each sample was examined to determine the effectiveness of this tech-nique in analyzing the correlation between precipitates and IATs in mitigating AGG.

Results and Discussion

Susceptibility to AGG after SHT for a sample with no IAT (S1) and several other samples that were given an IAT prior to SHT is demonstrated in Figure 2. The FSW is de-noted by the hourglass-shaped region in the images. More detail regarding the FSW and spin-forming process can be found in a re-cently published NASA report [2]. AGG was most prevalent near the advancing side of the weld, which is the boundary on the left side of the FSW. Samples F1 and 144 HR exhibit

some suppression of AGG at the t/4 region but still display areas with large grains. However, sample B1 reveals significant sup-pression of AGG at t/4 and is consider the most successful of the IATs shown.

The various samples analyzed in this study revealed the effectiveness of insert-ing an intermediate annealing treatment (IAT) before the SHT. Because AGG pri-marily occurs during SHT, the IAT stage is necessary to produce both effective for-mation of the weld and continuous grain growth within the microstructure [6]. Conventionally, a greater number of pre-cipitate particles that are smaller in size are favorable in stabilizing the Al-Li mi-crostructure [3]. However, the evaluated samples exhibited less AGG with fewer precipitates and varying sizes and obvious changes in the precipitate distribution as a result of the IAT.

The material underwent the IAT at an ideal temperature and duration to allow for continuous grain growth in obtaining a stabilized microstructure. Samples F1, 144 HR, and B1 demonstrated the greatest suppression of AGG at the three evaluated temperatures. Each presented a varying de-gree of success, particularly at the t/4 loca-tion. Sample S1 was selected to represent the before IAT condition.

Using ImageJ software, the images cap-tured with the BSE detector on an SEM at 1000x were analyzed to determine the ef-fect of precipitate size and distribution in the mitigation of AGG. Each image was

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Figure 2. Micrographs of samples with thermal conditions after SHT (Adapted from [2]).

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measure specific aspects of the microstruc-ture (Figure 3).

Once the precipitate particles exhibited a clear, visible contrast to the background, the image was altered using the binary func-tion (Figure 4). This technique illuminated the Cu-rich precipitates, separating them from the surrounding Al matrix. Though the images originally exhibited some con-trast in the initial SEM image due to the varying atomic weights of the elements, a binary image was necessary for the soft-ware to identify pixels as particles (black) against the surrounding matrix (white).

The precipitates in each image were

thresholded using the maximum, mini-mum, brightness, and contrast functions, as shown in Figures 3 and 4. The image’s pixel size was then calibrated by identify-ing the known distance and unit of length (e.g. 50 µm), enabling the software to

evaluated using the “Analyze Particles” function. This study utilized the summary function’s data of precipitate population, average size, and area fraction (the per-centage of space the particles utilize). However, the results function has the capa-bility to output statistics for each individual particle, providing an exhaustive study of precipitate size and distribution for future research. The data output for one image of sample B1 at the t/4 region is presented in Figure 5.

After collecting data from all 10 sam-ples, the calculations of each sample’s pre-cipitate count, average size, and area frac-tion were compared to determine any trends from sample to sample. Depending on the sample’s thermal condition, the number of precipitates ranged from approximately 100 to 900 particles in each 90 x 70 µm image. The average area of each precipitate was between 0.3 to 0.9 µm2. Area fractions ranged from approximately 0.9 to 3.0 %, measuring the ratio between particles and

Ashle M. Page

Figure 3. ImageJ thresholding and scale functions.

Figure 4. Original, thresholded, and binary SEM images of sample B1 in ImageJ.

Figure 5. Precipitate data computed for sample B1 with ImageJ.

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the microstructure.

Summary

Through a comprehensive investigation of the microstructure of Al-Li alloy 2195, FSW was examined to analyze the impact of IATs on precipitate particles and suscep-tibility to AGG. BSE images were captured at the t/4 regions and post-processed with ImageJ software to quantify precipitate size and distribution. Samples that had un-dergone different IATs at varying times and temperatures exhibited significant progress in promoting continuous grain growth. Future research should investigate other ar-eas of the weld in a more exhaustive study.

Recovery annealing treatments such as IATs are effective in suppressing AGG. However, application of standard Zener drag concepts does not seem to explain the microstructural effect. The IAT alters the microstructure, including the precipi-tate particle size and distribution, which leads to improved stability during SHT. The impact of the IAT on precipitates was not quantified in prior research. Through this study, an analytical technique was developed to quantify precipitate popula-tion and distribution by measuring particle

the surrounding space. Figure 6 compares the population, size, and distribution of precipitate particles in samples S1, F1, 144 HR, and B1. Overall, the count, average size, and area fraction (% area) decreased in most samples as the temperature of the IAT increased. To test the reliability of the data, error bars represent the ranges between high and low values in each graph, measur-ing actual variation between samples with trends greater than the experimental error. Collected results from image analysis were also graphed along with trends of conven-tional theory concerning AGG and thermal treatments. Samples S1, F1, 144 HR, and B1 followed the curve toward continuous grain growth as the temperature of the IAT increased, demonstrating trends similar to conventional theory.

Although the initial analysis appeared to contradict conventional wisdom con-cerning precipitate population and size, the data collected measuring the count, size, and area fraction do exhibit a common trend regarding suppression of AGG. As the temperature of the IATs increased, the samples began to undergo more continuous grain growth. Through this study, a tech-nique was successfully developed to quan-tify precipitate size and distribution within

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Figure 6. Example of data trends with respect to IAT at the t/4 region.

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and thresholding procedures. Precipitate distribution will also need to be compared with grain size to better understand the role of precipitate particles on AGG. [9]. Increased strength and ductility of mate-rials fabricated through the spin-forming process will ultimately lead to greater reli-ability and reduced cost in the manufactur-ing and operation of aerospace structures.

Acknowledgments

The author would like to acknowl-edge the mentorships of Wesley A. Tayon, Dr. Stephen J. Hales, Marcia S. Domack, Dr. Philip B. Bogert, and Dr. Fred R. DeJarnette, in addition to the research fa-cilities of NASA Langley Research Center, Hampton, Virginia, and sponsorship pro-vided by the NASA Langley Aerospace Research Student Scholars (LARSS) Program and North Carolina Space Grant.

count, size, and area fraction. Though a thorough correlation between precipitates and suppression of AGG has not been fully resolved, preliminary results suggest that there may be a correlation between the dis-solution of precipitates during the IAT and a reduction in the extent of AGG. The most effective IAT at suppressing AGG resulted in the smallest precipitate quantity, size, and area fraction of precipitates. This cor-relation may be due to the reduction in par-ticles providing a more favorable environ-ment for competitive or continuous grain growth during SHT.

Through the technique developed, fur-ther study of the impact of IATs on pre-cipitates may lead to greater suppression of AGG by promoting a stabilized micro-structure within the FSW. Solving the prob-lem of AGG will lead to increased strength and ductility within the FSW for structures fabricated through the spin-forming pro-cess. Future work will need to apply com-putational methods to standardize imaging

Ashle M. Page

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