My atempt at alloying antimony with lead

[sparkeyu]

well i had a pound of antimony i picked up at a gun show a couple years ago and decided to give it a try today
saw on here some others experiences, took about seven pounds of lead and added 6oz of tin and fluxed with
some bullet lube i had. broke up the antimony into six pieces and put into the pot and fluxed and stirred.
it started to dissolve and stirred some more, cant believe how easy it was. all dissolved in about 30 min.
will try this again for sure

[fiberoptik]

I picked up some little bottles of 95% tin/5% antimony for like $2/jar. I think it's a powder. Also some rolls of 50/50 solder. Haven't used them yet but I will. Just brought down my lead from Michigan.

[Drew P]

Yeah I read a lot of horror stories and bad advice from people who had never done it and in the end it was quite easy. Just place in lead, and stir. Dissolves quickly and easily. Done.
I did make sure to capture all dust produced from the shattering process which, again, was easy.
In case anyone is contemplating this just know that the melting point of antimony, while being ~1150°, is completely irrelevant because you don't need to melt it to alloy it. It dissolves.

[jmort]

^^^ I have never seen any "horror stories" here about antimony. With the easy availability of lead/antimony alloys, most don't want to waste time alloying antimony with lead. In fact, many/most are cutting the existing antimony content of their alloys. You max out around 16% "dissolving" antimony so there are limits on what you can do.

[sparkeyu]

Hard to get high antimony lead around hear at a good price. if my math is correct I ended up around 12 percent and was no harder than cutting ww 50/50 with lead. just wanted some hard cast for beowulf and 460 rowland.

[jmort]

From what I have read the mix maxes out around 16% if you merely "dissolve," as opposed to melt the antimony, so I am wondering if you have a true alloy, or a "swirl/parfait." Unfortunately we no longer have the Antimony Man as a resource.

[typz2slo]

No antimony around here. I had to buy a couple 70/30 bars from Rotometals.

[jmort]

RotoMetals sells antimony and there is an interesting video in this link

http://www.rotometals.com/product-p/antimony.htm

[sparkeyu]

Im not sure but looked like it blended in quite well,ill check the hardness and see if it is uniform

[popper]

Sb does NOT alloy with Pb, period - always a 'mix/solution'.

[sparkeyu]

Popper do you think what I did is a viable alloy

[oso]

sparkeyu has a real alloy. Don't get discouraged by sarcasm and ignorance. For example Pb 90% Sb 10% is a eutectic alloy. I have exceeded 22% Sb alloyed in Pb. I do know Bill Ferguson, the late Antimony Man, once a young whippersnapper himself, taught me that Sb and Sn form an inter-metallic compound that facilitates alloying the Sb with Pb.

[Drew P]

Hey jmort I never said the horror stories were in here, but some questionable advice was. And since when was any of this hobby about saving time or availability? I hear Walmart sells already loaded ammunition maybe that's some advice that will save you some time. Sorry to offend you so much with my green shoes. Wasn't trying to give advice, just trying to help anyone who was in my position by distilling some of the theoretical with some real world experience first hand by me, and I sprinkled in some cautionary bits just in case also. No big deal. Carrion.

[typz2slo]

This is a very true statement. After doing PMI analysis on many samples I have seen different percentages of antimony in the same sample from taking readings on the top and bottom.


Sb does NOT alloy with Pb, period - always a 'mix/solution'.

[Chris24]

All my COWW ingots have slightly different amounts of antimony. Some are more frosty, some are more shiny. My last batch had so much, I had to mix some old batches in with it to bring the hardness down. It might have been a higher tin content than usual, too.

[montana_charlie]

it started to dissolve and stirred some more, cant believe how easy it was. all dissolved in about 30 min.
will try this again for sure
Did your alloy temperature reach 1167 degrees?

[Pooch]

Have always used Lyman #2 for all of my bullets. After paying premium price for 70/30 @ rotometals for a long time I decided to start using 40:1 for all of my sub-sonic loads e.g. .45 Colt, .44 Special & .38 Special. I was just wasting my money by using Lyman #2 in my sub-sonic loads. I like dealing with Rotometals as their products are pure & clean. I just found that the harder bullets weren't necessary for everything.

[popper]

inter-metallic compound NOT a true technical alloy. It is a good alloy for what we want and what we call it. Sparkeyu - it has the proper ingredients for our use, you can change it to various % to fit your needs.

[GunStuff]

... Snip... Nice to see one month old smug members who have so much to teach the forum. You really think anything in your post is ground-breaking or arcane?
You are not a real welcoming gentleman. Why spew dross at a new member who wants to have a conversation about our hobby?

[jmort]

I take exception to the following:

"Yeah I read a lot of horror stories and bad advice from people who had never done it and in the end it was quite easy. "

He clarified that he read the "horror stories" elsewhere, somewhere out there, but further stated that the forum contained "questionable advice." So in this respect, i.e. the "horror stories," I will stand corrected.

[sparkeyu]

Temp was not 1167 it was around 700. All I know is it looks real consistent and measures 22bn from numerous boolits I cast from it. all I can say to the skeptics is to give it try
Thanks to all ,I learn a lot on this forum

[jmort]

This is not an issue of skepticism. This is issue of wanting to get uniform results when combining lead, tin, antimony. This is what you should consider:

After doing PMI analysis on many samples I have seen different percentages of antimony in the same sample from taking readings on the top and bottom.

[fredj338]

well i had a pound of antimony i picked up at a gun show a couple years ago and decided to give it a try today
saw on here some others experiences, took about seven pounds of lead and added 6oz of tin and fluxed with
some bullet lube i had. broke up the antimony into six pieces and put into the pot and fluxed and stirred.
it started to dissolve and stirred some more, cant believe how easy it was. all dissolved in about 30 min.
will try this again for sure

Bought at a gun show, how do you know what it even was? Pure antimony has a much higher melt point that lead, why it is diff to alloy. In already alloyed form, like hardball, Lino, etc, it melts & alloys quite easily. If I need antimony in an alloy, I buy something like Lino to blend with. You probably bought an ingot of Lino or monometal.

[BattleRife]

Sb does NOT alloy with Pb, period - always a 'mix/solution'.

And what is an alloy if it is not two metals mixed and/or in solution?

157980

Taken from http://download.springer.com/static/pdf/860/art%253A10.1007%252Fs11669-011-9952-4.pdf?originUrl=http%3A%2F%2Flink.springer.com%2Fa rticle%2F10.1007%2Fs11669-011-9952-4&token2=exp=1452648047~acl=%2Fstatic%2Fpdf%2F860%2F art%25253A10.1007%25252Fs11669-011-9952-4.pdf%3ForiginUrl%3Dhttp%253A%252F%252Flink.spring er.com%252Farticle%252F10.1007%252Fs11669-011-9952-4*~hmac=5f503b4df98da9883d6d7989e0b2184e7053dbc89c 0dc77bd72a165c010a6c90

The binary phase diagram for lead and antimony shows a eutectic at 16.75%, meaning that lead with 16.75% (by weight) of antimony will form a single phase, homogeneous solution when liquid (above 252°C). It is entirely reasonable to expect that this amount of antimony will dissolve into liquid lead at any temperature above this point. Larger amounts of antimony will dissolve into lead at higher temperatures.

If you have more than 16.75% antimony then you will get a slush of liquid alloy + solid antimony at temperatures between 252° and the liquidus. If you have less than 16.75% antimony you will get a slush of liquid alloy + solid lead in that window.

Below 252°C (and certainly at room temperature) it does appear that the alloy will segregate into two phases, one lead-rich and the other antimony-rich. At that 16.75% Sb content there should be equal amounts of each. These two phases will be intimately mixed together, like the alternating patterns of iron carbide and ferrite in a steel, and must absolutely be considered an alloy.

[montana_charlie]

Temp was not 1167 it was around 700. All I know is it looks real consistent and measures 22bn from numerous boolits I cast from it. all I can say to the skeptics is to give it try
Thanks to all ,I learn a lot on this forum
1167 degrees is the melting point of antimony.

Using the numbers you supplied, the alloy you made is essentially 84/4/12, which is the same ratio that is found in linotype.
Did your antimony look like a poured ingot ... or like the picture?

https://upload.wikimedia.org/wikipedia/commons/thumb/5/5c/Antimony-4.jpg/220px-Antimony-4.jpg

[jmort]

Taken from http://download.springer.com/static/...2a165c010a6c90

So this is saying you can get to 16.75% antimony. Interesting.

This is interesting as well:

Microsegregation in the Lead-Antimony Alloys 1
http://jes.ecsdl.org/content/100/1/1.full.pdf

[typz2slo]

pb 75.10

sn 8.29

sb
16.61






pb 85.42

sn
4.42

sb
10.16




This is the results from XRF analysis of a 1lb sample cast from a lyman ingot mold. The readings on top were from the top and the second set of readings were from the bottom. The percentages of both shots add up to 100% so everything was identified. The surfaces were scraped clean to ensure good clean readings. This sample was sent from a member here on the site. I have seen the the mixed readings a above in about 5-10% of the samples I have analyzed.

[alfloyd]

"Did your alloy temperature reach 1167 degrees?"

So how do the guys get copper to dissolve into lead when it is at 700 deg F.?

Lafaun

[Don Fischer]

I'd read a long time back, somewhere, that antimony won't mix with lead. But it does with tin and the antimony in lead is surrounded by tin that mix's with the lead. Id that true?

[popper]

BulletF - a technical alloy is a molecular change to the metallic structure which is homogeneous throughout the sample. you want your 4041T to be the same throughout the sample and it DOESN'T change over time.
For our use, Pb/Sb/Sn is called an 'alloy'.

[oso]

BattleRife, Thanks for the Good Info! Note that on the phase diagram you posted the top scale is weight percent antimony and the bottom scale is Atomic Percent Antimony. The 16.75% figure is from the bottom scale, the percent by weight Sb is 10 - 11% (top scale) for the Pb/Sb eutectic (that is to say the alloy composition with the lowest melting point.)

[oso]

Taken from http://download.springer.com/static/...2a165c010a6c90

So this is saying you can get to 16.75% antimony. Interesting.

This is interesting as well:

Microsegregation in the Lead-Antimony Alloys 1
http://jes.ecsdl.org/content/100/1/1.full.pdf

Hey jmort, forget that part about 16.75% antimony, forget that I said I got to 22% antimony in lead, but remember that RotoMetals says their Super Hard Alloy Ingot is 30% Antimony and 70% Lead.

[BattleRife]

BattleRife, Thanks for the Good Info! Note that on the phase diagram you posted the top scale is weight percent antimony and the bottom scale is Atomic Percent Antimony. The 16.75% figure is from the bottom scale, the percent by weight Sb is 10 - 11% (top scale) for the Pb/Sb eutectic (that is to say the alloy composition with the lowest melting point.)

Whoops!! You are correct, I didn't notice that the top and bottom scales were different.


Taken from http://download.springer.com/static/...2a165c010a6c90

So this is saying you can get to 16.75% antimony. Interesting.


Actually it says you can achieve any percentage but you need more heat for any mix other than 11% (by weight). For example to get a 50-50 mix of antimony-lead you need to take it up to about 495°C to get complete melting. But as I stated earlier (and as the article you linked goes into very good detail on) the antimony will start to segregate when you drop the temperature, and the final alloy ends up being non-homogenous, with a mix of antimony rich islands in a matrix of eutectic composition. But it is still an alloy.

[oso]

Excellent discussion. If we understand this then we understand what is happening through the slush phase when it is occurring.

[KYCaster]

This is not an issue of skepticism. This is issue of wanting to get uniform results when combining lead, tin, antimony. This is what you should consider:

After doing PMI analysis on many samples I have seen different percentages of antimony in the same sample from taking readings on the top and bottom.



I Googled PMI and found lots of stuff from Personal Mortgage Insurance to Post Mortem Interval, but nothing related to metallurgy.

Could you tell me what it means please?

Jerry

[typz2slo]

PMI Positive Material Identification. I manage the inspection department of a chemical plant and we use an XRF gun to identify the alloy components of piping, fittings and welding rods when building and repairing equipment. Its the same tool that the scrap yards use. In my industry its PMI and here its known as XRF analysis. Sorry for the confusion. Its just a different language for the same thing. That was my mistake. Sorry about that.

I have been using my device to analyze samples that members from the site have sent me. I have been keeping a spreadsheet and can show what has been discussed about ingots being homologous vs concentrated areas of antimony rich islands in the alloy. I am not a metallurgist and not as familiar as some on here about the alloy matrix and do not claim to be one but try to provide information to other members about their alloy. I analyze and report as accurately as I can as to what the samples contain so who sent it to me will know what they have and then they can determine the best mix for what they are casting.




I Googled PMI and found lots of stuff from Personal Mortgage Insurance to Post Mortem Interval, but nothing related to metallurgy.

Could you tell me what it means please?

Jerry

[BattleRife]

I have been using my device to analyze samples that members from the site have sent me.

How big is the window on your X-Ray Fluorescence unit? I would guess that regions of Pb-Sb eutectic would give pretty consistent results in your analysis, as the segregation of the phases is so fine you will be capturing large swathes of each phase. But with non-eutectic compositions if your window is smaller than a couple of millimeters you could easily land in areas that were rich in one constituent or another. This photo, taken from the paper jmort linked to, clearly shows that segregation of antimony (fine black lines and shapes) has resulted in antimony-rich areas on the scale of about 1000 microns (1mm).

158325

[KYCaster]

PMI Positive Material Identification. I manage the inspection department of a chemical plant and we use an XRF gun to identify the alloy components of piping, fittings and welding rods when building and repairing equipment. Its the same tool that the scrap yards use. In my industry its PMI and here its known as XRF analysis. Sorry for the confusion. Its just a different language for the same thing. That was my mistake. Sorry about that.

I have been using my device to analyze samples that members from the site have sent me. I have been keeping a spreadsheet and can show what has been discussed about ingots being homologous vs concentrated areas of antimony rich islands in the alloy. I am not a metallurgist and not as familiar as some on here about the alloy matrix and do not claim to be one but try to provide information to other members about their alloy. I analyze and report as accurately as I can as to what the samples contain so who sent it to me will know what they have and then they can determine the best mix for what they are casting.



Thanks for the reply.

Jerry

[montana_charlie]

the antimony will start to segregate when you drop the temperature, and the final alloy ends up being non-homogenous, with a mix of antimony rich islands in a matrix of eutectic composition.
In the case of a single bullet starting to cool in the mould, that process seem likely to leave a 'shell' of segregated antimony on the bullet's surface ... which cools first amd fastest.

Is that what makes the 'frosty' part?

[BattleRife]

A frosty appearance comes from having large grain sizes, which in turn is a product of slow cooling. That's why your first bullets out of a cool mould are shiny, as the mould has a lot of capacity to quickly conduct heat away from the cooling bullet. As the mould gets hotter it can no longer take that heat away, so the cooling rate drops, and the lead grains get bigger.

With Pb-Sb alloys the lead has a strong tendency to solidify first. The crystals also have a tendency to grow fastest in certain directions, and those directions are at well-defined directions relative to each other, very often perpendicular. So a crystal will start growing as a slender rod, in a straight line. Then a branch will form off the side and start to grow as a slender rod in a direction 90° to the first one. This goes on until a very large part of the lead is consumed, then the antimonal phase starts to solidify by forming islands in between the rods of lead. This is called a dendritic structure and is quite common in primary solidified materials.

Here is an image of dendrites in an exotic cobalt-based alloy, taken by electron microscopy:
158451

So you don't really end up with a shell-and-core effect, it's more like raisins distributed throughout a muffin.