Analysis of aluminum alloy sample Aurora TX

ASSESSMENT COMMENTS ON METALLURGICAL ANALYSIS AURORA, TX ALUMINUM SAMPLE Anonymous, PA, 2008
1.1    Introduction
In 1973, samples from a mass of aluminum were sent by John F. Schluesser to several metallurgical labs for analysis. From the photographs it appears to be an irregular chip-like mass approximately 3 cm x 2 cm by 1 cm. In the published documents, it is claimed to have been received from Bill Case of Dallas, TX on June 19, 1973. Mr. Case reportedly found it beneath 4 inches of soil in a field in Aurora TX, lodged against a limestone rock face.
Figure 1. Photographs of aluminum sample obtained from B. Case, 1973. Numbers on top scale correspond to 0.1 inch. As this was an amateur investigation, there is no documentation of proof that the sample came from this location. Furthermore, as its provenance is associated with Mr. Schuessler and Mr. Case, both associated with studies of paranormal phenomena and hoaxes, it is highly questionable that this sample was found in the location stated. There is no information regarding the age of the sample. Nonetheless, the sample did exist in 1973, and was subjected to seemingly valid metallurgical analysis. It is on these results that we comment.
1.2    Analytical Results
Figure 2. Sketch of sample and its sectioning into multiple samples for analysis (Schuessler documentation 1973)
The sample was apparently sectioned and sent to several analysis labs. The results are tabulated below.
1.2.1    EDAX Analysis Robert J. Danmeller, Marion Russo, (organization not given) In the documentation, it states this organization was given sample #2, but from their sketches, however, it appears they may have been sent sample #1. Analysis was conducted using SEM imaging and EDAX composition analysis.Runs 1-4 were taken from the face of a surface exposed by the sectioning, and correspond to the interior of the sample. EDAX specra indicates strong Al peak with 2 secondary peaks labeled Fe. Run 5 was taken from an exterior surface region.
Material    Peak    Actual (keV)    Run 1interior    Run 2interior    Run 3interior Run 4interior    Run 5surface    Reported(keV) Mg    Ka1    1.254    --    --    --    --    -- Mg    K-edge    1.303    --    --    --    --    -- Al    Ka1    1.487    4000*    4000*    4000*    4000*    4000    1.45 (Al) Al    K-edge    1.560    --    --    --    --    -- Si    Ka1    1.740    --    --    --    --    304    1.70 (Si) Si    K-edge    1.840    --    --    --    --    -- S    Ka1    2.308    --    --    --    --    -- Pb    Ma1    2.346    --    --    --    --    194    2.35 (Pb) Bi    Ma1    2.423    --    --    --    --    -- S    K-edge    2.470    --    --    --    --    -- Cl    Ka1    2.622    --    --    --    --    122    2.65 (Cl) K    Ka1    3.314    --    --    --    --    161    3.30 (K) K    K-edge    3.608    --    --    --    --    -- Ca    Ka1    3.692    --    --    --    --    168    3.70 (Ca) Ti    Ka1    4.511    --    --    --    --    615    4.50 (Ti) Ti    K-edge    4.965    --    --    --    --    137    4.95 (Ti) Cr    Ka1    5.415    --    --    --    --    -- Mn    Ka1    5.899    --    --    --    --    -- Cr    K-edge    5.989    --    --    --    --    -- Fe    Ka1    6.404    100*    200*    1400*    100*    217    6.40 (Fe) Mn    K-edge    6.538    --    --    --    --    -- Fe    K-edge    7.111    --    30*    200*    --    66    7.05 (Fe) Ni    Ka1    7.478    --    --    --    --    -- Cu    Ka1    8.048    --    --    --    --    -- Cu    K-edge    8.980    --    --    --    --    -- Zn    Ka1    8.639    --    --    --    --    -- Zn    K-edge    9.661    --    --    --    --    -- Pb    La1    10.55    --    --    --    --    54    10.55 (Pb) Bi    La1    10.84    --    --    --    --    -- Table 1. Peak intensities from EDAX analysis on metallurgical sample taken at 4 interior locations (Runs 1-4) and one location on the exterior surface (Run 5). Data in rightmost column are peak locations reported, along with the material they were indexed to. (*) indicates estimate from EDAX screen shots
Energy dispersive X-ray (EDAX) is useful for identifying the presence of elements in an alloy, but quantitative composition measurement requires careful calibration to known standards. Nonetheless, there is no observable Cu or Zn found anywhere in the sample. This suggests the sample is a pure Al-Fe alloy, with some surface contamination.
1.2.2    MDRL Laboratory Ronald A. Weiss, Sr. Group Engineer, McDonnell-Douglas Research Laboratory The analysis was conducted by J.E. Holliday using X-Ray fluorescence and soft X-Ray spectroscopy. It is stated they were given sample #1
Material    XRay fluorescence    Soft X-Ray spectroscopy Al    0.95    0.98 Fe    0.05    0.01-0.02
Table 2. Composition of metallurgical sample determined by x-ray analysis
In this analysis, Holliday reports the presence of cavities often associated with shrinking, and an overall microstructure consistent with solidification processing. He identifies small crystals of Fe-Al intermetallic compound. It is noted they are more numerous near the outer surface than in the interior. The percentage of Fe is higher in the XRF signal because it samples the enitre cut surface, while the soft X-ray spectroscopy samples only a 1mm x 3mm spot on the cut surface, initially located in the interior of the sample. The second phase inclusions are described as needle-like, but their sizes are not given.
1.2.3    Spectro-Chemical Research Laboratories 3300 West Lawrence Avenue, Chicago IL 60625, Bernard B. Hauser
This analysis by an independent lab appears to have been ordered by Art Bethke, (Motorola?). It is not clear if this sample is from the same where this sample was cut from. Bethke later reported the composition most closely matched the 2011 alloy. The standard composition range for this alloy is shown for comparison the Table below.
Material    Sample    Alloy 2011 Al    balance    balance Cu    5.68    5.0-6.0 Zn    0.02    0.30 max Fe    0.38    0.7 max Si    0.26    0.40 max Mn    0.02    (<0.05) Ni    --    (<0.05) Mg    0.01    (<0.05) Ti    trace    (<0.05) Pb    --    0.20-0.6 Bi    --    0.20-0.6 Table 3. Measured composition of metallurgical sample, with commercial aluminum alloy 2011 shown for comparison.
These results indicate the presence a large amount of copper, along with other components that suggest this is likely a commercial alloy, in contrast to the other analyzed samples.
1.2.4    Antsas Technical Services - EDAX analysis Antsas Technical Services, Another analysis via EDAX was conducted in 1994, again showing 2 Fe peaks in addition to the primary Al, and an absence of other materials. It is unknown if this data is from the same material analyzed in 1973. The analysis indicates the sample is 99.5% Al, with 0.5% Fe.
2.    DISCUSSION Aluminum alloys containing significant concentrations of Fe have been prepared and stuided in the laboratory at least since 1916[1]. Precipitates of the AlFe3 intermetallic compound were identified in these alloys as early as 1919[2]. By the mid 1970's there were several hundred papers in the literature concerning Al-Fe as an alloy, owing to its interest as in intermetallic forming system[3], high temperature structural applications, and a creep-resistant high temperature conductor[5]. Such alloys consist of an aluminum matrix into which are dispersed iron aluminide particulates, that form a creep resistant microstructure enabling it to maintain structural integrity at elevated temperature[5]. The class of structural intermetallics compounds that includes iron aluminides (Fe3Al, FeAl), along with related systems nickel aluminides (Ni3Al, NiAl) and titanium aluminides (Ti3Al, TiAl) posess many attractive properties for high temperature structural applications. The aluminum rich composition favors formation of protective Al2O3 in oxidizing environments, low density, high melting points, and high temperature strength[6], and it is predicted they are the most likely to replace superalloys in future applications. A key challenge is overcoming the brittleness of pure single phase intermetallics at low temperatures and developing improved fabrication techniques.
Given the low solubility of Fe in Al and their widely different melting temperatures, producing a bulk alloy of these materials is difficult. An overall composition of Al0.95Fe0.05 can be prepared via solidification from a high purity melt above 700C containing Al and Fe in these quantities, or via powder metallurgy whereby Fe and Al particles are milled together in a mechanical attrition process, then sintered to form a bulk compact. In the metallurgical analysis of 1973, it is mentioned that the sample has large grains with needle- like iron-rich strucutures. This is suggestive of a solidification process where Fe-rich liquid segregates ahead of dendritic or cellular/ columnar solidification and forms extended iron-rich strucutres and precipitates in the interdendritic/intercellular spaces. Powder metallurgical microstructures typically would consist of a more equiaxed microstructure with small Al grains interspersed with compact AlFe or Al3Fe intermetallic particulates.
Figure 3. Fe-Al Phase diagram. Sample composition is on the aluminum- rich end at Al0.95Fe0.05.
3.    CONCLUSIONS Technical From the available metallurgical analysis documentation of 1973, it appears     The sample is an alumunum matrix composite with overall composition Al0.95Fe0.05, with extended or needle-like Fe-rich structures, likely an iron-aluminide intermetallic phase.     Given the composition and microstructure this sample must have been produced in a well-controlled metallurgical process, such as in a laboratory.     The capability to produce this material has existed since 1920, but this composition would not have been widely available until sometime after World War II. By 1973 it would have certainly been available to someone with R&D connections in the aluminum or aerospace industries.
Relation to location of discovery     The claim is that this metal sample was recovered from an 1897 'debris field' in Aurora TX, but there is absolutely no proof that this sample is truly from this location. The sample discovery was not properly documented and changed hands several times thus making it useless for further study.     Although Al-Fe alloys have been produced in research quantities throughout most of the 20th century, they are not available commercially, and therefore highly unlikely to have been deposited by normal human activity in a rural area such as the location alleged.     If the sample were truly collected from a debris field (for which there is no proof) it is almost certain that additional amounts of material would remain at the site. These fragments, likely in much smaller sizes, perhaps 1 mm or less, would probably lie within the top few cm of soil or embedded in rock faces. This alloy would also be likely to remain relatively stable underground for decades.     Although they may not be locatable by 'hobbyist' metal detectors it is likely that archaeological excavation with fine particle fragment collection techniques could discover additional samples of this alloy-- if it exists in a debris field of fine particulates.     If new samples could be found (with proper on-site scientific documentation), the crucial step would be to examine in detail the composition and microstructure to ascertain with more certainty how it might have been produced. Additional analysis to estimate the time this material was in contact with the soil would be needed.
4.    REFERENCES 1.    O. Bauer and O. Vogel, "Aluminium-zinc alloys", Internationale Zeitschrift fur Metallographie, v 8, n 3, p101-178, (1916). 2.    P.D. Merica, R.G Waltenberg, J.R.Freeman, "Constitution and metallography of aluminium and its light alloys with copper and magnesium", Bulletin of the American Institute of Mining Engineers, n 151, p1031-1049, (1919). 3.    S. Nasu, U.Gonser, P.H. Shingu, Y. Marakami, 57Fe Mossbauer spectra in splat quenched Al-0.5, 1, 3 and 5 at% Fe alloys, Journal of Physics F (Metal Physics), v 4, n 2, L24-28 (1974). 4.    A. Olszowka-Myalska, J. Szala, J. Cwajna, Characterization of iron aluminides formed in situ in an aluminium matrix compositMaterials Characterization, v 56, n 4-5, p379-83 (2006). 5.    R.W. Westerlund, "Effects of composition and fabrication practice on resistance to annealing and creep of aluminium conductor alloys", Metallurgical Transactions A (Physical Metallurgy and Materials Science), v 5, n 3, (1974). 6.    J.R. Davis, Heat Resistant Materials, ASM Handbook, 1997.
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I suppose you are saying ? moon men ?
Actually, there is a large Aluminum fab lines in operation - many engineers have samples and junk. The other possibility is an early satellite breaking up around there and over head... breakup trail. Also to the West is White Sands. There they were sending rockets and missiles skyward and blowing them up. Wonders ever cease - the winds would blow it Eastward.
I, being of high tech and of the Missile world for many years know that target missiles fly high and when exploded do star bursts.
I suspect the sample was from a logical source but the finder and such were not thinking of airplane or missile material. American or German in those days.
Martin
Martin H. Eastburn @ home at Lions' Lair with our computer lionslair at consolidated dot net TSRA, Endowed; NRA LOH & Patron Member, Golden Eagle, Patriot's Medal. NRA Second Amendment Task Force Charter Founder IHMSA and NRA Metallic Silhouette maker & member. http://lufkinced.com /
snipped-for-privacy@mailinator.com wrote:

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On Feb 2, 9:33 pm, snipped-for-privacy@mailinator.com wrote:

SNIP
I think you are making WAY too much out of finding that someone had some pieces of aluminum alloy analyzed and found only iron by SEM-EDS and X-ray fluorescence. If I had not found your other post I would have assumed that you were pulling our legs.
Now, if you go to the Aluminum Association and look up their wrought alloy composition tables (the Teal Sheets) at: http://www.aluminum.org/Content/NavigationMenu/The_Industry/Industry_Standards/Tealsheets2006.pdf then you will find that there is a whole series of 8XXX iron containing alloys registered for commercial use. See page 20 of the pdf file (or page 12 of the printed version). Alloy 8079 was registered in 1969. It contains 0.7 to 1.3% Fe and 0.05 to 0.30% Si. Alloy 8021 (registered in 1992) contains 1.2 to 1.7% Fe and 0.00 to 0.15% Si..
The 8079 and 8021 alloys are used commercially for aluminum foil in packaging applications.
See "Industrial Development of Non-heat Treatable Alloys" http://www.materialsaustralia.com/Materials_Forum/Vol28/INV%206.pdf
and also see "The Combination of Film & Foil - Still Up To Date" (which mentions 8006, 8014, and 8079) http://www.alucontainer.org/media/Film_and_Foil.pdf
and also Alcoa European mill products catalog (which mentions 8006, 8011, and 8079) http://www.alcoa.com/mill_products/catalog/pdf/specialties/en/foil_EN.pdf
Pittsburgh Pete
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So we don't know where it came from.

Nor this one.
Furthermore, as its

AHhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhhh ....

So what were they in fact sent?
Analysis was conducted using SEM imaging and EDAX

Meaningless arm waving and technobabble given the preceeding.

Well then, I guess that this meeting is over.
I deal with credulous goofballs frequently and this posting is typical of what one gets from the classic interweb crank. When one strips away the references, lab names, technobabble one is left with the fact that two anonymous "things" were analysed. Hardly a factoid worthy of killing electrons.
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On Feb 2, 9:33 pm, snipped-for-privacy@mailinator.com wrote:

Some additional comments. The other post is on alt.alien.research and is titled "Reassessment of Aurora TX 1897 Aluminum Alloy"
The Acrobat .pdf data file is on the web at:
http://www.mufon.com/famous_cases/Aurora%20Texas%20Crash%20Part%201%20MUFON%20Case%20File.pdf
and also at:
http://www.scribd.com/doc/1618203/9202-submitter-file1-Al-Intermetallic-03
Page 51 of the 199 page data package shows a chemical analysis from Spectro-Chemical Labs in Chicago for their Lab No, 10756. The handwritten note on page 50 points out that the results are closest to the 2011 alloy, but that this sample does not contain the lead (Pb) and bismuth (Bi) specified for that commercial alloy. (These elements are present as particles that make the material easier to machine). The sample reportedly has 5.68% copper (Cu) which indicates that it is a completely different alloy than the other samples analyzed by SEM- EDS.
The following table is similar to Table 3 of the post but also adds the reported lead content, which is NOT consistent with a 2011 alloy. The second column shows the specified composition range on page 2 of the printed version for the Teal Sheets. Note "a" indicates that some elements are not explicitly specified but are to be reported as "other" with a maximum of 0.05% each and 0.15% total. See: http://www.aluminum.org/Content/NavigationMenu/The_Industry/Industry_Standards/Tealsheets2006.pdf
The third column shows the specified composition for the older version of this alloy (Army Air Force Specification 11330). It was reported on page 813 of the 1948 edition of the ASM Metals Handbook for the nominally Al - 5.5 Cu- 0.5 Pb - 0.5 Bi alloy then known by the trade name of 11 S alloy.
Element        Lab No. 10756        2011 Spec     AAF Spec 11330 Cu        5.68            5.0 - 6.0        3.5 - 6.0 Zn        0.02            0.0 - 0.3        0.0 - 0.3 Fe        0.38            0.0 - 0.7        0.0 - 1.0 Si        0.26            0.0 - 0.4        0.0 - 0.8 Mn        0.02            a        0.0 - 1.0 Ni        none            a        - Mg        0.01            a        0.0 - 0.8 Ti        trace            a        - Cr        0.02            a        0.0 - 0.25 Pb        0.03            0.0 - 0.6        0.2 - 0.7 Sn        0.02            a        - Al        rem            a        rem Bi        not reported        0.2 - 0.6        0.2 - 0.7
Others (each) a    -            0.0 - 0.05    0.0 - 0.05 Others (total)    -            0.0 - 0.15    0.0 - 0.15
Now, SEM-EDS analysis typically can only detect an element if more than 0.1% is present in the sample. Comparing a spectrochemical analysis with an SEM-EDS analysis is comparing apples and oranges. There is no reason to conclude that "this is likely a commercial alloy, in contrast to the other analyzed samples". The other samples may also have contained commercial levels of impurity elements, but they would NOT have been detected. They may have been something as mundane as the material used on this planet for making cigarette wrapper foil.
Pittsburgh Pete
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On Feb 2, 9:33 pm, snipped-for-privacy@mailinator.com wrote:

SNIP
The MUFON Acrobat .pdf data file of the Aurora data is on the web at: http://www.mufon.com/famous_cases/Aurora%20Texas%20Crash%20Part%201%20MUFON%20Case%20File.pdf
I could not find the metallurgical assessment on the MUFON site but did find the pdf file corresponding to the sci.engr.metallurgy newsgroup post of Feb 2 at: http://www.scribd.com/doc/1618203/9202-submitter-file1-Al-Intermetallic-03
What are these materials? Are they commercially available now? Were they commercially available in 1973? How easily could they have been processed to produce the "debris" samples reportedly found at the "crash site"?
In the metallurgical assessment chemical compositions of the alloys were not stated in consistent units. The analyses from MDRL and Anastas were in atomic percent while the Spectro-chemical analysis was in weight percent. Weight percent is used in commercial specifications, so I will use it.
Results for the two main elements found, iron and copper can be summarized as follows:
Lab % Iron % Copper MDRL 9.8 - Spectro-chemical 0.4 5.7 Anastas 1.0 -
There are three completely different samples!
First consider the MDRL 9.8% iron sample. Now, this is suspiciously close to being exactly ten percent. An aluminum alloy containing nominally ten weight percent iron is a "master alloy" commonly used as a convenient way of adding iron during the production of other aluminum alloys. Iron melts at a much higher temperature than aluminum, so it would not be added directly in commercial production. It's sort of like ordering a vanilla latte at a coffee shop. They will not stir your drink with a vanilla bean - they just will add a splash of vanilla syrup.
See Table 1 of the Key to Nonferrous Metals article on "Master Alloys for Aluminium Alloys: Part Two:" http://www.key-to-nonferrous.com/default.aspx?ID=CheckArticle&NM 5 A master alloy with nominally ten percent iron has both Aluminum Association designations (H2810, H2811) and European Community designations (CEN AM-92600, 92601). The Aluminum Association designations are contained in a document called the Gray sheets: http://www.aluminum.org/Content/NavigationMenu/The_Industry/Industry_Standards/graysheets.pdf H2810 was submitted in 2005 by the EAA (European Aluminium Association). The Aluminum Association only began the process of standardizing master alloys back in 1973. See: http://www.aluminum.org/Content/NavigationMenu/The_Industry/Master_Alloys/MagicArticle.pdf Therefore it is not clear how long ago such an alloy could have been purchased off the shelf in the US. However it melts at a much lower temperature than pure iron and could easily have been recast to produce a debris sample.
Second, consider the Spectro-chemical sample containing 5.7% copper. This corresponds to a commercial alloy called 2011 (or its predecessor, 11S). You can buy 2011 from Alcoa under the trade name of Toolrite: http://www.alcoa.com/gcfp/catalog/pdf/alcoa_toolrite_2011.pdf 2011alloy also contains 0.2 to 0.6% of both lead and bismuth. These elements are added to produce particles that make this material much easier to machine than most other aluminum alloys. Alloy 2011 was registered in 1954, and 11S is in the 1948 Metals Handbook. Now, both lead and bismuth are much denser than aluminum. They also are insoluble in liquid aluminum. If you tried to remelt a 2011 alloy, then the lead and bismuth would wind up dropping to the bottom of the container, just like an oil and vinegar salad dressing tends to separate. The Spectro-chemical analysis found only 0.03% lead, consistent with remelting of a chunk of 2011 alloy.
Third, consider the Anastas sample containing 1.0% iron. The intentional use of iron in aluminum alloys is an inexpensive way of making stronger material for foil. This type of commercial alloy was around before 1973. It melts at a slightly lower temperature than pure aluminum, so it would be easy to recast to produce "debris".
If you go to the Aluminum Association and look up their wrought alloy composition tables (the Teal Sheets) at: http://www.aluminum.org/Content/NavigationMenu/The_Industry/Industry_Standards/Tealsheets2006.pdf then you will find that there is a series of 8XXX alloys. See page 20 of the pdf file (or page 12 of the printed version). Alloy 8079 was registered in 1969. It contains 0.7 to 1.3% Fe and 0.05 to 0.30% Si. The 8079 alloy is used commercially for aluminum foil in packaging applications. See "Industrial Development of Non-heat Treatable Alloys" http://www.materialsaustralia.com/Materials_Forum/Vol28/INV%206.pdf Also see the Alcoa European mill products catalog: http://www.alcoa.com/mill_products/catalog/pdf/specialties/en/foil_EN.pdf
There also is an older "potluck" alloy called 8112 that was registered back in 1954. All the composition limits in this specification are maximums, so you can make it from whatever recycled stuff you have around, like the vegetable soup served in a diner. You are allowed to have up to 1% silicon, or iron, or zinc. Now, 8112 alloy is used for highly sophisticated products like license plates. See the "US License Plate Technology overview" at: http://www.jrwald.com/Downloads/TagWhitepaper.pdf More specifically 8112 Aluminum has been in state purchasing documents for license plate stock from Virginia, New Jersey, and for Pennsylvania: http://www.dgsweb.state.pa.us/comod/Contracts/CN00014159.pdf
Pittsburgh Pete
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