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[*] posted on 27-5-2018 at 19:16
Nickel, Iron, and Molybdenum from Mu-Metal (Hard Drives)


After conducting a search of the forum and wiki for information regarding the purification of primarily nickel from Mu-metal alloysSource 1, I found that there were no procedures that have been written. Having 154.7 grams of this alloy myself, I would like to try my hand at this.

For anyone with a few hard drives sitting around they are an excellent source interesting metals. Potentially just from these pieces of metal a nickel, iron, and molybdenum can be extracted. Aside from that, the magnets contain neodymium (my next project), the platters contain small amounts of platinum, and so on.

Mu-metal contains between 77-80% nickel, 12-16% iron, 0-5% copper, 0-2% chromium,0-5% molybdenum, and trace amounts of silicon. Source 1 It is contained within modern hard drives as a shielding around neodymium magnets (about 50 grams/hard drive).

Here are my thoughts so far;

Considering that both nickel and iron metal are both magnetic at room temperature, they may be separated from the non-ferromagnetic metals like chromium and copper.

The whole alloy can be dissolved using HCl and H2O2, leaving behind the silicon.

Iron and nickel have very similar properties and will be difficult to separate from one another.

With what acids will nickel and iron not react and react? Sources online have not been specific.


Source 1: http://www.sciencemadness.org/smwiki/index.php/Mu-metal

USC10K900.jpg - 191kB download.jpg - 15kB

[Edited on 28-5-2018 by VSEPR_VOID]




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[*] posted on 27-5-2018 at 19:27


Magnetic separation ain't going to help you separate elements of an alloy. Your choices are going to be either some kind of wet chemistry approach or selective oxidation at high temperatures (which is what is done to refine steels.)

I think you need to as a first step dissolve in a strong acid. Then you can selectively precipitate out the species you are after.
I am doing a similar experiment extracting vanadium from a pile of rusted screwdriver bits. I used HCl because that is what I have on hand. I have not yet decided on a procedure for separating the vanadium from the iron: I need to do some more reading.

There are procedures out there for separating chromium and nickel from iron -- look up the dichromates from stainless steel threads. The interesting target I think is the molybdenum. Good luck!




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[*] posted on 27-5-2018 at 19:38


Quote: Originally posted by j_sum1  
Magnetic separation ain't going to help you separate elements of an alloy. Your choices are going to be either some kind of wet chemistry approach or selective oxidation at high temperatures (which is what is done to refine steels.)


I was not clear when I mentioned separation based on ferromagnetic, or lack-there-of, properties, I meant the precipitation of metals from solution (created by dissolving the metal in acid) using aluminium, and removing the nickel and iron metal using a magnet. This would leave with nickel and iron metal.

It might be possible to allow the iron to oxidize, perhaps by using a solution of salt water, then again use a magnet to removed the nickel.


I too agree that Mo seems like a interesting target. I unfortunately know nothing about its chemistry. Could you recommend a text on the topic?




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[*] posted on 27-5-2018 at 20:08


Nickel forms a complex with ammonia, iron doesn't. You can use that to separate the two ions. Copper(II) ions can be reduced to insoluble copper(I) salts using iodide ions, ascorbic acid, etc.

Using a ferromagnetic approach sometimes doesn't work, as the metal powder that precipitates is sometimes a mix of atoms interlocked in a crystal lattice.




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[*] posted on 27-5-2018 at 20:21


I have a lot of these metal plates and have thought about doing this before and stopped because it looked like A LOT of work with the potential of small returns and creating a lot of toxic waste. The chromates thread is a good start but also separating the Ni and Cu is going to be a PITA as well.

I looked into separating the neodynium from the mags as the recovery rate was extremely low (about 1-2% yield) in many cases so I decided against the whole experiment.

Is this just to practice separation or to obtain usable reagents?

[Edited on 5-28-2018 by RogueRose]
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[*] posted on 27-5-2018 at 20:21


My Mo chemistry is limited to a short experiment dissolving Mo wire in various acids with and without peroxide. I forget the results but I can look them up. Oh, and I have also used Mo compounds in testing for phosphates.

I am sure that there are good texts you could use though.




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[*] posted on 27-5-2018 at 21:13


Quote: Originally posted by ninhydric1  
Nickel forms a complex with ammonia, iron doesn't. You can use that to separate the two ions. Copper(II) ions can be reduced to insoluble copper(I) salts using iodide ions, ascorbic acid, etc.

Using a ferromagnetic approach sometimes doesn't work, as the metal powder that precipitates is sometimes a mix of atoms interlocked in a crystal lattice.


Is the complex insoluble? I have seen photographs of a nickle complex of ammonia but there is no precipitate present.

The copper reduction is a good idea, do you have a procedure that you know works? Would that also reduce iron?

That fact about interlocking atoms in crystal lattices is interesting.

Quote: Originally posted by RogueRose  

I have a lot of these metal plates and have thought about doing this before and stopped because it looked like A LOT of work with the potential of small returns and creating a lot of toxic waste. The chromates thread is a good start but also separating the Ni and Cu is going to be a PITA as well.

I looked into separating the neodynium from the mags as the recovery rate was extremely low (about 1-2% yield) in many cases so I decided against the whole experiment.

Is this just to practice separation or to obtain usable reagents?


You should try it. Considering the alloy is mostly nickel it is not a bad source of the metal. It also might be economic considering that nickel nitrate is 12 dollars for about 60 grams online. 100g is about 10 dollars on ebay (not considering bulk orders of 1 pound which are 30 dollars).

My goal is to extract a pure Ni salt, Fe salt, and Mo salt for use in making ferrocyanides. I am hoping for a yield of between 80 and 100g of nickel metal equivalent.




My experimentation so far


23.4g of Mu-metal was added to a 600ml beaker. To it 150 ml of 31.45% HCl and 100ml of 3% hydrogen peroxide. The solution was gently heated to 80C with some stirring. There evolved a large amount of gas and the solution turned urine yellow. This color is probably due to iron (III) chloride in solution.

[Edited on 28-5-2018 by VSEPR_VOID]

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[*] posted on 27-5-2018 at 22:13


Vsepr-void:

I will be very surprised if you have more than a trace of nickel in that solution and what is there may be from the nickel-plating the bracket has.

The brackets pointed to in the first post are part of the magnetic circuit of the neo magnets and are usually made from soft iron (almost pure iron). They hold the magnets in place and conduct the magnetic flux between the rear faces (the opposite face to the ones next to the coil). Soft iron is used as it has a high permeability and high saturation. Mu metal would saturate.

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[*] posted on 27-5-2018 at 23:55


Quote: Originally posted by wg48  
Vsepr-void:

I will be very surprised if you have more than a trace of nickel in that solution and what is there may be from the nickel-plating the bracket has.

The brackets pointed to in the first post are part of the magnetic circuit of the neo magnets and are usually made from soft iron (almost pure iron). They hold the magnets in place and conduct the magnetic flux between the rear faces (the opposite face to the ones next to the coil). Soft iron is used as it has a high permeability and high saturation. Mu metal would saturate.



Than why is it stated on the wiki that the brackets are 77% Ni metal?
http://www.sciencemadness.org/smwiki/index.php/Mu-metal

Update on the reaction: The solution is still yellow and the mu-metal's coating as not dissolved but the insides nearly have completely. Almost like a penny placed in hydrochloric acid, dissolving the zinc but not the copper.




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[*] posted on 28-5-2018 at 01:30


Quote: Originally posted by VSEPR_VOID  




Than why is it stated on the wiki that the brackets are 77% Ni metal?
http://www.sciencemadness.org/smwiki/index.php/Mu-metal


Possibly because it was written by someone who was mistaken.

You have a solution that contains some of the metal.
If you add excess ammonia then the iron will fall out as a mixture of hydroxides/ oxides etc and nickel will remain in solution as a purplish blue complex (much the same colour as the copper ammine complex).
So you can do that test now and settle the matter.
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[*] posted on 28-5-2018 at 01:33


That is very disappointing. Someone should change the wiki at once! The solution is only yellow. If it is just iron it may not be worth doing anything with it.



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[*] posted on 28-5-2018 at 01:37


Quote: Originally posted by VSEPR_VOID  
Quote: Originally posted by wg48  
Vsepr-void:

I will be very surprised if you have more than a trace of nickel in that solution and what is there may be from the nickel-plating the bracket has.

The brackets pointed to in the first post are part of the magnetic circuit of the neo magnets and are usually made from soft iron (almost pure iron). They hold the magnets in place and conduct the magnetic flux between the rear faces (the opposite face to the ones next to the coil). Soft iron is used as it has a high permeability and high saturation. Mu metal would saturate.



Than why is it stated on the wiki that the brackets are 77% Ni metal?
http://www.sciencemadness.org/smwiki/index.php/Mu-metal

Update on the reaction: The solution is still yellow and the mu-metal's coating as not dissolved but the insides nearly have completely. Almost like a penny placed in hydrochloric acid, dissolving the zinc but not the copper.


I have given you my reasoning why I think its not Mu metal, I suggest you ask the author of the wiki why he thinks it is Mu metal. No real reference was given.

Perhaps the plating on the bracket (possibly electro less nickel/phosphorous alloy) did not dissolve and the inner iron is dissolving.

When I have used HCl to dissolve parts of a magnetron. I got impatient and added H2O2 then heated the solution. That was a bad idea it gave off a lot chlorine and the heat probably decomposed any H2O2 that was left. It probably would have been better (used less acid and peroxide) to not have heated the solution. Perhaps that’s why your plating did not dissolve.

I thought nickel chloride was green even in HCl. Of cause you will soon be able to definitively say if there was significant nickel in your bracket.

I just checked the colour of a few crystals of nickel chloride in HCl and it is green.

[Edited on 28-5-2018 by wg48]
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[*] posted on 28-5-2018 at 02:13


Yes, its strange that that the solution is still yellow. It shows no colors of nickel or cobalt. I think you might be right, in which case I am deeply disappointed.



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[*] posted on 28-5-2018 at 03:33


Quote: Originally posted by VSEPR_VOID  
That is very disappointing. Someone should change the wiki at once! The solution is only yellow. If it is just iron it may not be worth doing anything with it.


It is worth adding excess ammonia solution to a little of the solution in order, once and for all, to find out if the stuff you have made has nickel in it
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[*] posted on 28-5-2018 at 06:57


The last time I tried to separate Ni from Fe using ammonia failed horribly.
It did nothing but make the area pungent.
For some reason little to no nickel dissolved.
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[*] posted on 28-5-2018 at 10:55


I have no idea what you're referring to. VSEPR here is trying to extract some potentially useful and exotic metals from a metal alloy, and none of what you have said will give him more information about his current experiment. [Edit by j_sum1 -- Refers to troll posts later pruned from thread]

Back to the topic, it might be just iron. Besides Canadian nickels, there are rarely any commonly available alloys with even 50+% nickel in them.

Reducing iron(III) to iron(II) won't form a precipitate because both are soluble in water. Copper(I) salts are not soluble in water regardless, which makes the reduction method for separating out copper work.

I have tried this using colorless iodine tincture (no free I2 in solution) and it does separate out copper as copper(I) iodide to some extent, but I happened to run out of the tincture and had to put it off for another day.


[Edited on 28-5-2018 by j_sum1]




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[*] posted on 28-5-2018 at 14:20


An Update On Reaction Progress: The solution has turned a darker yellow and the case has no dissolved, only the inner metal. I hypothesize that that case is made of something like cobalt and the insides steel or iron.

The case is resistant to HNO3, and HCl with H2O2 and heating.

Does anyone know a way to test the yellow solution for other metal ions to determine if it is steel or some other alloy?




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[*] posted on 28-5-2018 at 14:52


IIRC woelen mentioned something about adding H2O2 to determine the presence of chromium. If there is chromium present, it should turn into a violet-blue color.





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[*] posted on 28-5-2018 at 15:39
http://www.sciencemadness.org/talk/


I will try that. I am hoping at this point I can at least get some nice ferric chloride out of this. The casing might be cobalt so that might be the best new target for this project.

Edit: After doing more research I found that the original claim on the SM wiki that the articulator's NdFeB bracket (it should be noted that the actual magnet is coated in nickel) is composed of Mu-metal originated from an non-cited claim on Wikipedia.

An hour in the library will save you 3 in the lab.

I still have another 130g of these brackets. If I can discover the composition of the acid resistant coating, and of the solution produced by dissolving the internal metal in HCl, then the project may still be salvaged.

Potentially from this I may be able to salvage 80-120g of iron (relative to the salt) and also what ever metal is coating them.

Additionally there are also the magnets to consider. I plan on taking this up next. If you are going to take apart of hard drive to get the magnets, you might as well also find a use for the other parts.

[Edited on 29-5-2018 by VSEPR_VOID]




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[*] posted on 29-5-2018 at 01:59


Quote: Originally posted by VSEPR_VOID  

I still have another 130g of these brackets. If I can discover the composition of the acid resistant coating,

[Edited on 29-5-2018 by VSEPR_VOID]

Nickel is remarkably resistant to acids. I have a coin sitting in sulphuric acid % which as been "dissolving" for months. It's still there, you can read the embossed lettering.

Nickel is also a very plausible coating for the brackets.
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[*] posted on 29-5-2018 at 02:03


Quote: Originally posted by unionised  
Quote: Originally posted by VSEPR_VOID  

I still have another 130g of these brackets. If I can discover the composition of the acid resistant coating,

[Edited on 29-5-2018 by VSEPR_VOID]

Nickel is remarkably resistant to acids. I have a coin sitting in sulphuric acid % which as been "dissolving" for months. It's still there, you can read the embossed lettering.

Nickel is also a very plausible coating for the brackets.


Have you tried dissolving it in another acid. At this point I am considering either boiling strong NaOH solution or aqua regia.




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[*] posted on 29-5-2018 at 02:06


Quote: Originally posted by VSEPR_VOID  

I still have another 130g of these brackets. If I can discover the composition of the acid resistant coating,

[Edited on 29-5-2018 by VSEPR_VOID]

Nickel is remarkably resistant to acids. I have a coin sitting in sulphuric acid % which as been "dissolving" for months. It's still there, you can read the embossed lettering.

Nickel is also a very plausible coating for the brackets.
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[*] posted on 29-5-2018 at 03:48


Quote: Originally posted by unionised  
Quote: Originally posted by VSEPR_VOID  

I still have another 130g of these brackets. If I can discover the composition of the acid resistant coating,

[Edited on 29-5-2018 by VSEPR_VOID]

Nickel is remarkably resistant to acids. I have a coin sitting in sulphuric acid % which as been "dissolving" for months. It's still there, you can read the embossed lettering.

Nickel is also a very plausible coating for the brackets.


I am considering trying either hot concentrated sodium hydroxide or aqua regia.




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[*] posted on 29-5-2018 at 06:43


As the guy who wrote the Mumetal page on the wiki, I feel the need to clarify than all the specs I've encountered about hard drives, say that the magnet brackets are Mumetal, and that mumetal is specified to be a nickel alloy. I too have several magnet brackets from various different types of hard drives, but unlike some people here, I haven't had any success dissolving anything: HCl gave me no reaction, adding a bit of 3% hydrogen peroxide gave me just a little rust, which, given that the alloy has iron, it should be expected, but other than than slight coloring of the solution, not much has happened. Sulfuric acid 30% didn't do anything. The only more corrosive stuff that I haven't tried are halogens, such as iodine or chlorine (as bleach).
There is another possibility as to why you didn't get the nickel coloring: your "Mu-metal" from the brackets is not true mu-metal. Years ago, when I took apart lots of hard drives, I found an old hard drive that had galvanized brackets and what I think it was a samarium-based magnet (well, some old but strong magnets). I found it odd why it won't be nickle plated like the rest of the hard drive magnet brackets, so I added a bit of acid, but not much happened. The next day the bracket was covered in rust in the area where I added the acid, which led me to believe that it probably wasn't a nickel alloy, but rather some iron alloy with high magnetic permeability, probably because it was cheaper, or because nickel alloys were more expensive back then.
Another possibility is that it is a nickel alloy, but for some reason only the iron dissolves. It's not the first time I've encountered nickel alloys that "rust". A few years ago I scavenged some heating elements that were very rusty, but when I placed them in HCl acid, the only thing that happened is that the rust was removed, while the metal wire did not dissolve, even after a few days of sitting in acid. Well, I assume the wire was nickel alloy, since if it was chromium alloy, some of it should have dissolved.




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[*] posted on 29-5-2018 at 09:04


If Ni in mumetal didn't dissolve in acids then why Ni in stainless steel do dissolve?
I tried dissolving SS in HCl previously and all Ni dissolved.




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