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Thread: Toughness Of Lead-tin-antimony Alloys

  1. #1
    Boolit Master
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    Toughness Of Lead-tin-antimony Alloys

    TOUGHNESS OF LEAD-TIN-ANTIMONY ALLOYS
    GEOFF CHAMBERLAIN
    When choosing which metal to use for a specific application, physical properties such as strength, hardness, ductility and toughness are often important. Toughness, defined as the ability to withstand shock loading, is commonly determined by the Charpy test (ASTM E23). This involves a pendulum breaking a standard specimen: the pendulum’s loss of energy from before-impact to after-impact is the toughness measurement.

    Toughness is a critical characteristic used by the military to compare the impact performance of specimens of armour plate. It has the potential to be similarly useful for comparing the expected behavior of bullets cast from various lead-tin-antimony alloys when they strike animals. Because I found little actual data on the toughness of these alloys, I decided to investigate the matter experimentally. In most respects the Charpy test was suitable for my experiments but I wanted to obtain a direct indication of specimen ductility. While ductility can be inferred from the ‘instrumented’ Charpy test it is not indicated by the simple mechanical version, and the instrumented version was beyond my intended scope. I therefore departed somewhat from the Charpy concept and chose to deform my specimens by a standard amount instead of just fracturing them. This still gave me a measurement of the deformation-energy required, but also enabled me to grade specimens as ductile if they deformed without cracking, intermediate if they cracked but retained considerable strength, and brittle if they fractured before reaching the standard amount of deformation.

    I developed a simple drop test device, shown in the first photograph. The large cast iron weight (partly-elevated and supported by a spring-clamp in the picture) is raised a suitable distance up the graduated slide then released to fall and strike the chisel, which rests against the side of a test specimen placed on an interrupted V block. The specimen, V block and chisel are shown in more detail in the second photograph.
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    The specimens were bullets cast in a Lyman 311466 mould: a standard commercial bullet mould readily available to other experimenters, and which easily produces large numbers of physically-identical cast specimens of suitable proportions for testing. Consistent axial location of each specimen was achieved by resting the shoulder at the end of the gas check rebate against the edge of the gap in the supporting V-block. This gap was 10 mm wide. The chisel tip was flat and 2.5 mm wide. The mass of the drop-weight could be varied between 1.5 and 6.5 kg (1.5 shown in photograph), and the drop-height could be varied from zero to 30 cm. The toughness measurement was simply equal to the potential energy of the weight when suspended at its drop-height, since all of this energy was subsequently converted to kinetic energy then absorbed in deforming the specimen. The effective anvil mass was maximized by clamping the test device in a large industrial vice bolted to a 16 mm steel bench-top.

    The standard amount of deformation I applied is shown in the first photograph below. Drop-height and -mass were adjusted to give an 8.5 mm dimension across each specimen after deformation, unless fracture occurred first. The specimen shown in the calliper was classified as ductile. The second picture shows an intermediate specimen, which developed a tensile crack directly opposite the chisel. The third picture shows some brittle failures: when deformed to the 8.5 mm dimension the two parts were almost separated, and could have been broken by finger pressure.

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    I investigated the effects of three variables on alloy toughness: heat-treatment, percentage of antimony, and having a low tin-to-antimony ratio versus equal amounts of tin and antimony in the alloy. Heat-treatment consisted of holding a sample for one hour at a selected temperature between 175 and 240 degrees Celsius, then water-quenching.

    The first experiment involved a wheel-weight alloy of about 0.2% tin and 2% antimony, remainder lead with a minor amount of arsenic. The alloys will be described by their percentages of tin and of antimony, so I will refer to this as 0.2/2 alloy. Physical analysis was not available, so all alloys were identified indirectly by simultaneous use of three methods: calculation based on their ingredients; the alloy’s liquidus temperature; and the hardness of air-cooled samples. In the absence of physical analysis, reported compositions should be considered approximate. All specimens of each alloy were cast in a single batch from a single pot of alloy. For each hardness level a sample comprising fifteen specimens was aged at ambient temperature for two weeks after casting or heat-treating, before testing. Five specimens from each sample were hardness-tested using a Lee tester, and as many of the other ten specimens as necessary were impact-tested at various energy levels until the required deformation measurement was achieved.

    The effect of heat-treatment on 0.2/2 alloy is shown by the chart below. In all of the charts that follow ductile results are shown as circles, intermediate results as triangles, and brittle results as squares. The lowest-hardness sample was always air-cooled and the highest-hardness sample was as hard as I could make that alloy by simple oven heat-treatment and water-quenching.

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    Toughness initially increased with increasing hardness, but a peak was reached at about 19 BHN and beyond this hardness, toughness declined.

    In the second experiment four fairly commonplace low-tin bullet-casting alloys having different antimony contents (0.2/2, 0.9/4, 2/6 and 2/13) were compared. Results are shown on this chart.

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    The greatest peak toughness, 7.5 Joules, was achieved by the 4% antimony alloy. Both 2% and 6% antimony alloys had less peak toughness than this, and the 13% antimony alloy had little toughness regardless of heat-treatment. In all cases peak toughness seemed to occur at a hardness close to 19 BHN.

    For the third experiment three of the four low-tin alloys were compared with their pseudo-binary equivalents. A pseudo-binary alloy of lead-tin-antimony has equal percentages of tin and antimony. In such alloys substantially all of the tin and antimony are expected to combine to form the compound SbSn, so the alloy effectively is binary, or consists of only two substances: lead and SbSn (ignoring minor amounts of arsenic that may be present). The well-known Lyman No. 2 alloy, which would be called 5/5 under the notation used here, is pseudo-binary.

    The first comparison was between 0.2/2 and 2/2 alloys. Results are shown in the following chart.

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    Up to 17 BHN there was little difference in the toughness of the two alloys. Above 17 BHN the pseudo-binary alloy was both tougher and more ductile, reaching its toughness peak of 9 Joules at about 21 BHN - slightly higher than the low-tin alloy’s 19 BHN.

    The second comparison was between 0.9/4 and 4/4 alloys. Results are shown on this chart.

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    Once again the pseudo-binary alloy’s peak toughness was greater at 9.6 Joules, and was reached at a higher hardness (23 BHN) – the peak hardness achievable for this alloy. There were insufficient data points to determine whether there was a difference in ductility between the low-tin and pseudo-binary alloys.

    The third comparison was between 2/6 and 6/6 alloys. Results are shown on this chart.

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    As in both previous instances, the pseudo-binary alloy reached greater peak toughness (8 Joules) than the low-tin alloy but this time did so at only slightly higher hardness (20 BHN). As with the 4% antimony alloys, the pseudo-binary alloy’s peak hardness was lower. The pseudo-binary alloy was the more ductile of the two.

    Six main observations can be made from these results. First, appropriate heat treatment enhanced the toughness of all alloys tested except 2/13, which even when air-cooled was at the 19 BHN optimum hardness for maximizing toughness. (The toughness enhancement from heat treating the next-highest-antimony low-tin alloy, 2/6, was very small.) Second, an optimum antimony content for maximizing peak toughness seemed to exist at somewhere around 4% antimony for both low-tin and pseudo-binary alloys. Third, every pseudo-binary alloy tested demonstrated substantially (26-29%) greater peak toughness than a low-tin alloy with the same antimony content. Fourth, the pseudo-binary alloys may have been more ductile than the low-tin alloys. Fifth, increasing the antimony content may have decreased the ductility of the alloys. Sixth, each alloy’s ductility may have been decreased by heat treatment. More data would be required to confirm the last three of these points.

    If the fifth and sixth observations are valid, greater hardness, whether it is attained by antimony content or heat-treatment, comes at the price of reduced ductility. However the data suggest that ductility can be increased by increasing the tin content, up to the point where tin and antimony contents are equal.



    This report makes use of both theoretical and empirical information from F. D. Weaver, “Type Metal Alloys”, Journal of the Institute of Metals Vol. LVI No. 1, 1935, pages 209-240.

  2. #2
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    i am happy to see this as i have thought this for some time.

    this probably should be stickied.......

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    Boolit Master
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    Quote Originally Posted by grumpy one View Post
    TOUGHNESS OF LEAD-TIN-ANTIMONY ALLOYS
    GEOFF CHAMBERLAIN

    However the data suggest that ductility can be increased by increasing the tin content, up to the point where tin and antimony contents are equal.

    Yep. This is what I found.
    Evaluate everything you read for safety and use common sense.

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    Boolit Master Ricochet's Avatar
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    Very interesting!
    "A cheerful heart is good medicine."

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    Boolit Mold
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    Talking testing

    It is definately interesting and thank you for doing the testing

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    Boolit Designer 45 2.1's Avatar
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    Interesting data. It would be more interesting with several more alloys with the same tests conducted with air-cooled, water dropped and oven heat treated boolits of each. There are some startling differences between some alloys and the hardness condition when you do this.
    45 2.1

    Knowledge without understanding is a dangerous thing. For a little knowledge entices us to walk its path, a bit more provides the foundation on which we take our stand, and a sufficient amount can erect a wall of knowledge around us, trapping us in our own ignorance.

    Never sleep, never die

    Knowledge is easy to get, but worthless if you never use it. However the info is free, so the only person you have to blame is yourself if you chose not to use the information.

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    Smile

    It would also be fascinating to see what happens with quenched boolits from the same batch tested at different times as they age harden and resoften.
    "A cheerful heart is good medicine."

  8. #8
    Boolit Master
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    What I am hoping will happen is that someone will offer to analyze samples of the test alloys. I can then snail-mail sample bullets to the volunteer, and when the results arrive, post the actual analysis as part of the report. That would enable me to commence the next phase: nailing down the optimum antimony content more specifically than "in the general vicinity of 4%". If I have an accurate starting point I can vary up and down relative to that point, and hopefully find the optimum to about one quarter of a percent - I'm confident about getting it within half a percent. With an accurate fix on the right antimony content, I can then check up on whether some other regularities really exist or are illusory. Ultimately the picture might become clear enough to get really ambitious and see what a touch of copper does to the story.

    Heat treatment has been the PITA part of the series of experiments, because results vary. Far too often I find that I've heat treated at two different temperatures but hardness results are almost identical, and occasionally even the reverse of what I'd expected. Since there is a two week delay between heat treating and testing, that has made the process extend over about 11 weeks so far, excluding the preliminary experiments and making the apparatus. I've also accepted BHN variances of up to 1.9 for individual samples. (Anything of 2 or over was rejected and a new sample prepared). Those high variance instances were relatively early in the series, and have been improved by better heat treatment technique, but it is still pretty rudimentary - even in May I've accepted variances of up to 0.9. I have established and posted both the air cooled and maximum heat treatment BHN numbers for all of the alloys I've tested, though a different heat treatment technique might increase the maximums a bit. The hardest individual specimen I tested (one of five specimens of 0.9/4 heat treated at 240 *C, which ended up with a variance of 1.9) only achieved 29.9 BHN.

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    Boolit Master Ricochet's Avatar
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    How precise and repeatable are the BHN measurements?
    "A cheerful heart is good medicine."

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    Boolit Master
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    Well, if you mean the actual tests I did, they were all done in the same place: by filing a flat on the side of the bullet, across the three drive bands nearest the base, and indenting the middle of the flat. I always tested five bullets of each alloy/heat treatment combination, plotted the mean hardness, and calculated the variance in hardness readings. BHN reading variances ranged from 0.3 to 1.9, with a mean of 1.0 across the 34 samples. The main issue was to ensure that the indentation wasn't too close to an edge, which messed them up royally, or observably out of round.

    I'm satisfied about two things: the Lee tester is the only one which actually applies the Brinell method; and my technique was somewhat consistent and generally complied with the Brinell/Lee instructions. However that doesn't mean that Lee built my particular instrument to specification, or that you can even make accurate Brinell tests on an object as small as a 30 caliber bullet. Furthermore reading the diameter of the indentation is fraught with difficulty with the apparatus involved. I've used a "real" Brinell tester, and Lee's el cheapo device isn't in that class in numerous respects. However I mounted the Lee microscope in a kiddie plastic microscope, and drilled the light-transmission hole in its stage to allow me to fit the Lee V-block to it. That gave me a stable microscope support and a stable specimen support that I could slide around. Nevertheless I found that if I went back to a month-old specimen it was not unusual to be able to read the indentation diameter differently by one Lee graduation, which seems a lot to me. Essentially I was probably getting better at using the apparatus over time. On this project alone I made well over 200 hardness measurements, and that is more than I'd made when I started it even though I'm rather prone to measuring hardness.

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    What I mean is, are the results repeatable enough if you were checking a piece of the same metal to make a meaningful differentiation between two samples that are, say 5% apart in BHN (as 1 sample reading 20 and another reading 19 or 21 would be.) I'm not sure small differences like that are meaningful in shooting, anyway. I'm not arguing that they aren't, I just haven't seen anything to prove that they are significant.

    Or if hardness variation is detrimental (which you would expect it would be at some point), how much does it take before you start seeing the real world shooting results change? There's fertile ground for experimentation, unless someone's already done work along that line that I haven't seen reported.

    Expectations are obviously critical to whether or how much it matters. If you're a competitive benchrester, you care about things like uniformed primer pockets and flash holes, precise neck thickness and concentricity, even how cases are indexed in the chamber, but if you're basically a plinker, you couldn't care less as long as it goes BANG. Same with boolit characteristics. Some will weigh every boolit and discard any outside a narrow range. Some will spin them to check for balance. Some will shoot anything that falls out of the mould and will fit into a case. Most of us are somewhere in between and have to decide what's worth paying close attention to and what's insignificant to us for our purposes (which may vary at different times.)
    "A cheerful heart is good medicine."

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    Seems to me there are two points here. First, I avoided the main point of your previous question because it was too hard: how much of the variability in hardnesses that I saw was due to actual variation in hardness of individual bullets within a heat treatment batch, versus how much was due to variability in hardness measurement even if all the bullets had really been of the same hardness? Second, how accurately can we expect to measure hardness, and how much does it matter?

    Regarding the first question, I noticed with the samples having the highest standard deviation of hardness, that drop test results were variable: I'd get insufficient deformation on a specimen, increase the drop height by a centimeter and try another specimen, and the deformation would be less than for the previous test instead of more. Of course the opposite happened too. This never happened with samples having a low standard deviation of hardness. So, the big standard deviations seem to have been associated with non-homogeneous samples.

    Turning to the second question, I've just pointed out that the overall average standard deviation I got, 1.0 BHN numbers, is an over-estimate of the variability due to hardness testing alone. However even with a standard deviation of 1.0, the statistical tables tell us that in my tests, 68% of individual test results would be within plus or minus one BHN of the correct mean for a large sample. So, at worst my measurements were within one BHN of correct two-thirds of the time, and most likely they were a bit better than that (because we know the reported S.D. (1.0) was boosted by non-homogeneous hardnesses of bullets in the same sample). How much does one BHN matter? Probably depends on how close you are to some limit, whether that means too hard or too soft. I think of it as analagous to powder charges: we should try to design our loads so that they aren't too close to some limit. If we have found by trial and error that we need a hardness of say 18 BHN to handle our load, but above 20 BHN our bullet-to-barrel fit becomes unmanageably critical, then we have a window of only 2 BHN to work in. If we are going to use up all of that and more just on the variability of our hardness measurements, we have chosen an unworkable loading condition. Get a better barrel, or reduce the load to a point where say 16 BHN is sufficient, so we have an operating window of 4 BHN instead of 2.

    I've probably tested everybody's patience with that esoteric explanation, especially since it's technically wrong: averaging the raw standard deviations of samples drawn from different populations is a no-no. I should have standardized the populations before averaging.

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    Now you have me wondering how the alloys we've been playing with made from WWs and babbit would stack up with the copper content.

    Felix swears by it and I've acheived pretty high velocities in the .223 with it and no leading or degradation of accuracy past 2400 FPS like with WW alloy./beagle
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    Boolit Master James C. Snodgrass's Avatar
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    I'm amazed at the variability of such small proportions can significantly effect the over all out come. I am very interested in any of your future experimentation on the matter . It seems we all have a infinite desire to achieve better results but some are much more adept at the means to read all the factors to attain these better results. Great job keep up the good work. James

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    Quote Originally Posted by beagle View Post
    Now you have me wondering how the alloys we've been playing with made from WWs and babbit would stack up with the copper content.

    Felix swears by it and I've acheived pretty high velocities in the .223 with it and no leading or degradation of accuracy past 2400 FPS like with WW alloy./beagle
    It is mostly felix's comments on this board that make me want to look into the copper issue, but I think proper scientific method requires that I tidy up the existing loose ends before starting a new program. I can't make any further progress at all, until or unless someone volunteers to provide actual analysis of the alloys I've tested so far (doesn't anyone know a friendly scrap merchant or metallurgy lab tech?)

    Then I think I should finalize the optimum antimony content, in the process acquiring some additional test data that may be sufficient to clarify the ductility trends. After that, copper is the next issue I'd hope to work on. A key question is whether there is interaction between antimony, copper and arsenic, which is why I want to start out with the optimum amount of antimony and experiment around that point rather than blunder about in a multitude of randomized constituents.

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    I'm glad that you're thinking about the copper alloys as well. Felix got me started on this track and I'm a firm believer especially for small caliber bullets in higher velocity applications.

    In fact, I think this may be an area of cast bullet alloys that even the bench resters have ignored.

    I guess one reason is because the alloy would be so hard to duplicate from batch to batch.

    I appreciate this study as I have always believed that an excess of antimony made bullets too brittle. Finally you're shedding some light on it.

    I'll be looking forward to further posts on this./beagle
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    @grumpy one:

    Do you always keep the relation Sb:Sn as 1:1?
    I ask because I read in the publication of Rick Kelter at LASC.ORG that
    Sn is responsible for age-softening. So he limits the tin-content at 2%.
    Here it's proved that the bullets keep their strength for years, the same with WW's with a still lower tin-content. What's about age-sofftening in Sb-Sn-1:1 Alloys?

    Or did I as a foreigner understand something wrong?

    Dirk - from a sunny germany

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    Boolit Master Ricochet's Avatar
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    Thanks for the clarifications, Grumpy! I'm really looking forward to your further reports!

    As for antimony/tin ratios, looking down tables of type metal compositions it seems there are a lot of 2:1 or 3:1 ratios.

    I've read that arsenic is put in shot to make it round up better while falling in the shot tower. That sounds to me like something that increases surface tension, likely not something we want a lot of in our boolits.
    "A cheerful heart is good medicine."

  19. #19
    Boolit Master on Heavens Range
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    Correct about arsenic. So does aluminum. Arsenic will actually make the boolit harder on its own merits, where aluminum won't in comparison. I have used either to make the boolit smaller in the shank area to make the shank small enough to fit checks. Arsenic is found in many babbits as well as enough to be had in magnum shot, whereas aluminum is found in aluminum stearate. ... felix
    felix

  20. #20
    Boolit Master
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    Quote Originally Posted by jahela View Post
    @grumpy one:

    Do you always keep the relation Sb:Sn as 1:1?
    I ask because I read in the publication of Rick Kelter at LASC.ORG that
    Sn is responsible for age-softening. So he limits the tin-content at 2%.
    Here it's proved that the bullets keep their strength for years, the same with WW's with a still lower tin-content. What's about age-sofftening in Sb-Sn-1:1 Alloys?

    Or did I as a foreigner understand something wrong?

    Dirk - from a sunny germany
    Hi Dirk,

    According to Weaver's paper, tin and antimony bond to each other to form the compound SbSn when both are present. If Weaver is correct, when you have both Sn and Sb, but less of the former, the Sb will preferentially bond with the Sn to form SbSn, and the surplus Sb will be in the form of Sb crystals. If the amounts are equal the Sb and Sn should ideally all be in combined form. The substance SbSn acts differently from Sb, but aside from noting it had much greater scratch resistance than Sb, Weaver didn't investigate its properties.

    Hence it is incorrect to think of Sn as existing in your alloy, whenever you have less of it than you do of Sb: what you have is some SbSn and some Sb. I haven't seen the LASC article you mentioned, but it appears the author is asserting that SbSn is responsible for age-softening, not that Sn is.

    At this early stage I have no information on age softening beyond the anecdotal reports in individual articles. Weaver did not investigate any kind of heat treatment of her typemetal alloys - I suspect it was completely unknown in 1935.

    Working on the premise that Weaver is correct, the common bullet alloys consist of lead with various proportions of Sb and SbSn crystals present. It is already apparent from the work I've done to date that a small proportion of SbSn provides substantially greater maximum toughness than an equivalent proportion of Sb crystals. On the other hand, Sb crystals provide a greater maximum hardening capability than SbSn crystals. The whole subject of age hardening and age softening is a mystery to me at the moment; I only treat anecdotal articles as a source of rumours and clues, not of facts.

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