Processing Black IC's - The wet way.

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samuel-a
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Processing Black IC's - The wet way.

Post by samuel-a » January 3rd, 2012, 6:11 pm

This method is also known as wet ashing, a highly dangerous process which should only be attempted by an experienced operator, with all of the proper safety gear and apparatus.
Otherwise, DO NOT follow this process !


----------------------

Jaun Nailed it in this post: Black IC's - a look inside
Since the method i used was unveiled and is indeed a very dangerouse process, i decided to share the entire process that i did, both to unveil the 'mystery' and make sure anyone trying this will keep himself SAFE.

The background to this process.
I my post, i said i had an: "ah ha moment"...
I was sitting in my lab and looking at my plastic buttle of conc' H2SO4, when i bought it, it was white, after several monthes it got very dark inside, that was the moment i remembered someone here on the forum mentioned that conc' H2SO4 strip the plastics off its elemental composing atoms, only to be left with black carbon, which gives this dark color.
At the time, i was busting my had around the black plastic type packages IC's and how to process them...
That was me 2+2 moment, since i have done wet ashing before with old filter papers...

So, i figured, if it takes couple months to "ash" the plastic in the buttle... imagine how fast will a HOT acid work...

I began experimenting and this is the process i came up with:

- IC's are covered with Conc' H2SO4 and the vessel is covered with watch glass (or condensation apparatus).
I came to learn that for each pound of IC's, i'll need a approx 1 liter of conc' acid.
Solution level should not exeed half the volume of the vessel !

- Slowly heated to 90° C (194° F) and left that way for 30 minutes.
This is a precautionary step to prevent too violent reaction and maybe a boilover.
The epoxy resin (Bismaleimide-triazine epoxy) will begin to disintegrate alsmost immediately.

- Then, heat is ramped up to 240°-250° C (464°-482° F) for one hour.
At which point, white Sulfur Trioxide fumes are noticble. I don't think i need to mention HOW DANGEROUS SO3 gas is. It is one step away from becoming sulfuric acid, all it needs is water, it can find them in you mouth and lungs!
The solution at this point is a black thick slurry and very hard to actually see any reaction, but it's happening.

- The solution is allowed to cool back down to ambient temp' while still on the hotplate (do not handle it while hot, reduce the risk of a mishap), this takes a good 2-3 hours.

At this point, all that's left in a solid state (other then carbon in a slurry and colloid form) are metals such as gold (wires), the silicon waffer and copper "skeltons" (in case memory chips are processed). I'll address that later.

- Slowly and carefully, water is added to the acid to double the volume.
I know what you are thinking, but, At this point, there's very little acid left to react with the water, but of course you can choose to do so the other way around.
Once diluted, is allowed to sit for 5 minutes or so.

- The bulk of the slurry is decanted slowly to a 5 gallon bucket, carefully leaving anything that had setteled in the vessel.
The process of dilution and decantation is repeated until all of the black carbon slurry is gone.
Of course, you will notice the gold wire, it's impossible not to!

Most of the wires will stay attached to the waffers, those that come loose, will quickly agglomerate. BUT, some will still be left to fly around, they do settle, but you must give them the chance to do so. This is why it is instructed to wait before decantation.
If you see any partially dissolved IC's, fish them out with a tweezers, wash them and throw to the next batch.

- The next step is dependant on which type of IC chips were processed.

In the case of N/S bridge and square IC's:
Mostly silicon waffers and gold wires are left, direct AR / HCl-Cl could be used.

In the case of memory chips, there will be a lot of copper along side the waffer/wires.
One can eliminate the copper with nitric acid or AP.
I chose to melt everything down to form a Copper anode.


Jaun mentioned in his post that he successfully used conc' Nitric acid, I find it a little bit scary, for even the slightest chance of producing an explosive compunds.
I might be wrong of course, but whan you think about it, hot conc' nitric is just as dangerous and can cost 5-10 times more then the sulfuric does.


I was very reluctant to discluse this process before due to 2 main reasons (never had inentions on selling it):

The first, is the obvious direct danger of utilizing boiling sulfuric acid...
i can't stress the safety issue enough.
Eye protection or a full face mask should be used while handling.
Long chemical resistand gloves should be weared at all time.
The process should be done in a fume hood or out side away from peoples and pets.
Extreme care sould be enforced while handling conc' H2SO4.
A bucket of sodium bicarbonate is recommended to have around, just in case.

The second reason, is the indirect waste hazareds.
As you probably realized earlier, this process produce a fair amount of of waste solution, one lb of chips may create up to a gallon of waste.
I consulted with two very smart folks on this subject, both of which holds a degree in chemistry (Lino1406 ans sucho).
We all concluded that the resulting waste solution will probably not hold any toxic organic/organosulfur/aromatic compounds and can be safely discraded to the drain.
The only treatment step that i do think should taken in this regards, is to place a sheet of steel to displace any Cu in solution.
Any input from you on the waste solution subject is more then welcomed.

I know this process can help A LOT of peoples here, but PLEASE, use all the safety measurements mentioned above.
It's not worth to loose the palm of your hand, your foot, sight or even your life for so and so grams of gold.

Hope this helps, DO share your thoughts, comments and experience.

----------------------

This method is also known as wet ashing, a highly dangerous process which should only be attempted by an experienced operator, with all of the proper safety gear and apparatus.
Otherwise, DO NOT follow this process !
Last edited by samuel-a on January 5th, 2012, 7:04 am, edited 3 times in total.
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Re: Processing Black IC's - The wet way.

Post by skippy » January 3rd, 2012, 6:16 pm

Bravo Sam, thanks for giving such a detailed example of the dangers.
And thanks for sharing such a potentially useful technique.

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Some photos from the different process

Post by samuel-a » January 3rd, 2012, 6:18 pm

SO1.JPG
SO12.JPG
SO123.JPG
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Re: Processing Black IC's - The wet way.

Post by philddreamer » January 3rd, 2012, 6:22 pm

Thank you Samuel!

Shalom! 8)

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Re: Processing Black IC's - The wet way.

Post by samuel-a » January 3rd, 2012, 6:26 pm

Thank you skippy and phil.

I reckon this process will be best suited, economy wise for N/S bridge chips and square IC's...
less for memory chips.

I'll leave my yields out of this post.
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Re: Processing Black IC's - The wet way.

Post by ericrm » January 3rd, 2012, 6:39 pm

wow thank you
i know i no good in english but im shock that you give your info just to keep everybody safe
i dont know you, but now i respect you at a higher degree than many poeple i know
thank you to be a man of honor
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Re: Processing Black IC's - The wet way.

Post by arthur kierski » January 3rd, 2012, 7:00 pm

please Sam,when you say conc sulfuric you mean 98% or half volume ,that is:50%h2o-50% 98%h2so4------- i understood full strenght 98%----no water
thanks
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Re: Processing Black IC's - The wet way.

Post by samuel-a » January 3rd, 2012, 7:07 pm

You understand right Arthur.
That is 98% concentration.
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Re: Processing Black IC's - The wet way.

Post by skippy » January 3rd, 2012, 7:08 pm

Sam, I know I'm going to give it a try, I have to see myself what your pictures show. Really cool.

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Re: Processing Black IC's - The wet way.

Post by Geo » January 3rd, 2012, 7:35 pm

thank you sam!! 8) this may have its dangers but it is much safer than what i was doing.

good job on the research and i just would like to say in general, job well done. :D
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Re: Processing Black IC's - The wet way.

Post by jaun » January 4th, 2012, 12:20 am

Hi Sam

Great post. Sorry for high jacking your post, but I thought you were never gonna tell your secret. :)

Like I said: I am using 55% nitric and it costs the same as cons. sulphuric here in SA.
And of course the safety issues is the same, it’s hot acid.
You got me worried about the explosive compounds now ??? :shock:
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Re: Processing Black IC's - The wet way.

Post by bswartzwelder » January 4th, 2012, 4:29 am

Thank you, Samuel. While I do not plan on using your method in the foreseeable future, I now knoe where to look. You are a class act.

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Re: Processing Black IC's - The wet way.

Post by hfywc » January 4th, 2012, 4:36 am

my hat's off to you...thank you kindly sam!
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Re: Processing Black IC's - The wet way.

Post by lazersteve » January 4th, 2012, 10:15 am

This method is very dangerous yet effective. Nice photos Sam.

I briefly mentioned the reagent for dissolving epoxy several years ago here on the forum:

Removing Epoxy Encapsulation

As I always say, there's not much that is new now days on the forum.

I will add that a much safer set up would be soxhlet extraction of the epoxy using this reagent. Trust me when I tell you that you don't want to be around 300+ degree celcius sulfuric acid with an open top reactor. A watch glass is not going to make much of a difference, if any. I have a few large ( 71/60 and 55/50 ) soxhlet rigs purchased especially for this type of reaction. Refluxing the water with the SO3 should help to reduce the fumes that escape the vessel and also allow for extraction of a much larger mass of epoxy with a given smaller quantity of concentrated sulfuric acid. Careful temperature control of the condenser and reaction vessel are critical to containing the SO3 gas safely. Proper handling and scrubbing of any off gases is also very important.

Careful heating and cooling of pyrex glass is critical when working with these extremely dangerous reagents (eg. hot concentrated sulfuric acid) at high temperatures. If your reactor breaks, there is a very high probability that you are going to get hurt. Fused quartz glassware would be a much better choice for use with this reagent and temperature.

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Re: Processing Black IC's - The wet way.

Post by samuel-a » January 4th, 2012, 11:12 am

lazersteve wrote:As I always say, there's not much that is new now days on the forum.
I guess so Steve...
That is why i never claimed the "invention" :mrgreen: , though, i must say, i have looked around for long time, both on google and here on the forum and never found your post or other information regarding the above process, maybe i didn't looked hard enough.

It seems like you didn't explored this avenue further since your old post in the link, or did you? maybe you could share some experience on the process.

Your tips and and safety notes are spot on. Also, I would very much like your input in regards to handling the waste solution.
I hate to think someone may harm the environment or get in trouble with the authorities over this promoted process.

Thanks
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Re: Processing Black IC's - The wet way.

Post by goldsilverpro » January 4th, 2012, 12:16 pm

Sam,

The process of using hot conc H2SO4 to break down organic materials is called "wet ashing" and it's been discussed a few times on the forum. What you are doing is nothing new. You've just applied it to something different. I've been using it since the 60s mainly for analytical work in small quantities. It's too dangerous to use for larger amounts (been there, done that). Even the small quantities that I normally used can be very dangerous if you don't know exactly what you're doing. I toyed with using it, at one point, to break down gold-bearing ion-exchange resins in large volumes, but dismissed it due to the inherent dangers.

Hot conc. H2SO4, is soooo dangerous that I am considering deleting this thread. I would strongly suggest that no amateur try it. There are better ways to handle those parts - incineration, for example.

Please don't make a video of this.
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Re: Processing Black IC's - The wet way.

Post by lazersteve » January 4th, 2012, 12:36 pm

Sam,

I for one was not set up to test the therory back in 2009 when I posted the link cited. I have tested it on a small scale myself though (see link below). The link is also not the only time the forum has discussed the use of hot sulfuric for dissolving epoxy. I found mention of the use of hot sulfuric acid as a reagent for dissolving epoxy numerous times via google around 2007 for the first time so I'm by no means claiming it's my 'invention' either. I knew of the post cited only because I remembered posting it myself. Other safer epoxy solvents have also been discussed, the one that caught my eye was known as Dynasolve 185 and is discussed in the post at the bottom of page one in this old thread:

Dynasolve 185 Epoxy Dissolver

A link in the above thread has a member who got his hands on a 55 gallon drum of the material.

Check out these other Dynasolve Products

For this type of scrap I currently prefer crushing and leaching with AR after the solder is removed with HCl as mention in the above cited thread from 2010.

I haven't explored the waste disposal aspects of the reaction as I feel there are safer and better routes to the same results.

Steve
Last edited by lazersteve on January 4th, 2012, 3:44 pm, edited 2 times in total.
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Re: Processing Black IC's - The wet way.

Post by Geo » January 4th, 2012, 1:06 pm

the post you linked had a reply from Quest42know above it.this is what i was using to break down the epoxy.it is very dangerous and i would never recommend anyone use a flammable liquid like that.even though it did break down the plastic,it did not dissolve it even when heated.before anyone throws a hammer at me,in my defense i would set my hot plate at the end of a 100' electrical cord with a GFI so i could basicly turn it on/off at a distance.the process sam describes IS very dangerous and i understand that any newcomer or beginner can see this as a way to process these cleanly without understanding the danger.but there are those among us that have and will deal with far worse and i for one think the post should remain as long as the dangers and safe handling are highly stressed.
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Re: Processing Black IC's - The wet way.

Post by samuel-a » January 4th, 2012, 1:08 pm

Chris, Steve

I tend to agree with you both.

As i said above, i was very reluctant sharing this process, and still am in disagreement (with myself) about it.

I never had any plans on posting a video of the process on youtube or at my website.
The main reason i did post it here, is that other member had reported his success with this process, so i felt kinda obligated to both share and warn.

If it's up to you Chris, i think it will be a wise on your part to delete this whole thread and the other posts made by the other member.
I will not be offended in any way. And pretty sure the other member will not too.

I know that we are all big boys and responsible to our own choices, but...
The very last thing i want is someone to get hurt by something i have suggested.

Again , Thanks for all of your comments.
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Re: Processing Black IC's - The wet way.

Post by butcher » January 4th, 2012, 2:41 pm

Sam, good post, but I see where someone who is not aware of dangers involved or Half ashed studied, could get hurt badly from this.

This is one process that has been discussed before but has not been recommended, and in fact has been discouraged, because of the dangers involved.

Sometimes it is better not to post some things.

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Re: Processing Black IC's - The wet way.

Post by glondor » January 4th, 2012, 2:42 pm

G.S.P. gave me a fairly strong warning about a year ago when I asked about wet ashing filters. I paid attention to it. Thanks Chris. Just a question before this thread goes away.

What would happen if sulfuric acid at working temperatures described in this thread came into contact with wood. Would the wood catch fire? Would you have a burning wood/ acid fire on your hands to deal with?

Can this process be done in a different manner such as it would be rendered safe? (safer) IE: over an extended period of time at room temps VS such high heat? Is high heat critical to wet ashing? Will room temp Sulfuric disintegrate the carbon over time.?
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Re: Processing Black IC's - The wet way.

Post by glondor » January 4th, 2012, 2:56 pm

Sam. Just a note. Too bad the process is so dangerous. Your results are beautiful, A recovery dream. The good stuff is right there for your eyes to see. Would be a great method for determining yield per pound except for the carbonized fleshy bits if you screw up.

A proper protocol and process could be developed but the cost for a home refiner would be very high. Good job on the experiment. Once again your results are fantastic. I fear someone is going to try this and get hurt.
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Re: Processing Black IC's - The wet way.

Post by hfywc » January 4th, 2012, 3:14 pm

quick question...to increase the concetration of battery acid to make it suitable for cell use, one has to boil down the acid to 1/3 of its volume, right? so, how is the danger different from wet ashing?
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Re: Processing Black IC's - The wet way.

Post by lazersteve » January 4th, 2012, 3:27 pm

hfywc wrote:quick question...to increase the concetration of battery acid to make it suitable for cell use, one has to boil down the acid to 1/3 of its volume, right? so, how is the danger different from wet ashing?
Sorry to say, but if you have to ask this question this method is not for you.

Be safe and use incineration followed by crushing.

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Re: Processing Black IC's - The wet way.

Post by Rodthrower18 » January 4th, 2012, 4:18 pm

Has anyone tried the MEK mentioned towards the bottom of the dynasolve thread? If I can find it locally I'll definitely post up my results. So far no luck, just a bunch of substitutes that equate to being ethyl acetate, which will evaporate much slower I just have no clue if it will actually WORK(doubtful since most substitutes do less work for more $).
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Re: Processing Black IC's - The wet way.

Post by philddreamer » January 4th, 2012, 4:37 pm

I tried some months ago MEK on PCB's trying to get rid of the solder mask, nothing happened. I have different black chips & IC's in MEK for the last 3 weeks, & they were not affected either.
I got my MEK from Home Depot.

I think I'll be incenarating.

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Re: Processing Black IC's - The wet way.

Post by Geo » January 4th, 2012, 5:04 pm

i didn't want to come out and say it but,the reply i made above concerned the use of MEK.i would BOIL the black plastic chips in MEK.WARNING:unless it is your intention to make a massively explosive situation do not ever attempt what i just said.it is dangerous and fool hardy.i have alot of land away from everything and only endangered myself and tried to minimize that danger as best as i could.the plastic would become soft but never did dissolve which was my objective.i still wound up incinerating the material anyway.
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Re: Processing Black IC's - The wet way.

Post by niteliteone » January 4th, 2012, 5:24 pm

lazersteve wrote:
hfywc wrote:quick question...to increase the concetration of battery acid to make it suitable for cell use, one has to boil down the acid to 1/3 of its volume, right? so, how is the danger different from wet ashing?
Sorry to say, but if you have to ask this question this method is not for you.

Be safe and use incineration followed by crushing.

Steve
The jenie is already out of the bottle :shock:
Deleting the post does not remove the infomation from those that have already seen it.

I feel that this needs a better explanation so those that do not understand can understand.

Some do not understand what hot concentrated sulfuric acid does to organic compounds. :shock:

I lack the ability to say it in a diplomatic way that most people can learn from without feeling scolded or worse, like wanting to try it just to see what I am talking about.
Can someone elaborate on what happens when things go wrong. Graghic details would also be good

I'm sorry Steve,
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Re: Processing Black IC's - The wet way.

Post by butcher » January 4th, 2012, 5:43 pm

I would not try to stuff any genie in a bottle, but I also would not like to hear of a member or anyone else, just reading a couple of lines on the intranet (our forum). Mangled for the rest of their life.

When we have safer and proven methods to use instead of wet ashing.

We could write up all of the procedures and all of the safety concerns, and all of the pictures of when and why things go wrong, why you should not do them in your basement, when making explosives, but that would not help a mother who's son read some of the instructions, disregarded warnings and crippled himself for life.

That is just how I see this, no argument I see your point mine just differs.

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Re: Processing Black IC's - The wet way.

Post by philddreamer » January 4th, 2012, 5:50 pm

I'm trying to post a pic of a person with an acid burn on his foot.

Phil

P.S. It worked.
Deleted the picture; added the link,

http://www.bing.com/images/search?q=aci ... ORM=IDFRIR

Sorry for the graphic depiction.
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If you are going to dream... DREAM BIG!!!
You may say that I'm a dreamer... but I'm not the only one!
"Paper money eventually returns to its intrinsic value --- zero." Voltaire (1694-1778)
The difference between a dream & reality is, a good plan!
WARNING: No "cartridge type" respirator will filter out nitric fumes, NONE!!!

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