Sciencemadness Discussion Board - Nickel Chloride From Nickel and Ferric chloride

Nickel Chloride From Nickel and Ferric chloride

NEMO-Chemistry - 10-6-2018 at 07:01

First i am sorry for another thread on this, i did one originally and despite my efforts cant find it! So i decided to let the Mod Gods sort it

.

Anyway a member on here has a blog i posted a link to recently, it has some experiments on making Nickel chloride. One of them mentions using Ferric Chloride acidified with HCl and a amine, apparently this was found to be a fast way to dissolve Nickel into Nickel chloride.

my own experience of this is, fast i think in this instance is highly subjective!!

At the moment i need/want nickel chloride from nickel flakes so i can plate nickel onto things. At some point i would like to isolate and purify the salt.

So here is my results, keep in mind i think i have a pic missing! seems to have been a camera mishap with a setting.

The amount of nickel used was roughly 1g, i didnt measure as it is simply a test to see if nickel would dissolve in ferric chloride.

In the other thread i cant find i did post the strengh of ferric chloride, but cant find it now. Anyway its about as strong as you can buy commercial ferric chloride.

I used around 50ml - 100ml, i dont remember and again did post it before. Again dosnt matter as you will see.

I acidified with 36% HCl, i used 2-3ml as the ferric chloride claimed it had some in anyway, the PH on paper indicated i hd dropped the PH to around 2

Because the blog said add a amine i am not sure why but i added 32% Ammonia, not much but this is what happened.

Not good!
So did it again and didnt add ammonia, 4 days later there was still a little nickel left

And what looked to be an extremely brown liquid! I didnt take a pic of it but it did look very much like this one with the exception there wasnt much orange stain around the top.

I decided to take some of this liquid and simply add water, i didnt measure the amount because i thought it had all failed, was adding water so i could see how dark it actually was. What i got was the following!

I am wondering if that is good enough to use to plate Nickel onto things? I can deal with chlorine and gasses by my normal pass through a one way valve and wash bottle technique.

The reason for asking is i tried to drop out any iron or maybe even the nickel chloride by complexing with Ammonia, however even adding two small drops from a pipette gave me the following

[Edited on 10-6-2018 by NEMO-Chemistry]

Before anyone jumps on me, i know this wasnt very scientific, but i did it as quick to see if i could get any Nickel chloride, Nickel is expensive and having tried various methods to dissolve into something i can use to plate with hasnt gone well.

I dont want to use Nitric, and sulphuric is just hard to get at the moment

[Edited on 10-6-2018 by NEMO-Chemistry]

CarlSagans_RayGuns - 11-6-2018 at 04:52

Nickel Chloride and HCl work great for an initial strike (super thin) layer but if you want any durability you may need a Nickel Sulphate bath. Here is the bath I am currently using:

Nickel Sulphate 250g L
Nickel Chloride 50g L
Boric Acid 30g L need pH 3.5 - 4.5

Here is a link to a pdf with some good advice and formulas.
https://www.nickelinstitute.org/~/media/Files/TechnicalLiter...

NEMO-Chemistry - 11-6-2018 at 05:07

first i got to get the nickel salts from nickel metal

.

But thanks for the info thats really handy. that seem alot of nickel sulphate, i only have 500g of nickel metal

CarlSagans_RayGuns - 11-6-2018 at 05:18

I use Nickel Oxide that I remove From old Ni MH batteries. I turn it to Nickel Chloride with HCl, then add baking soda to make Nickel Carbonate. Then Nickel Carbonate to Sulfuric acid makes Nickel Sulfate.

fusso - 11-6-2018 at 06:50

Quote: Originally posted by CarlSagans_RayGuns

I use Nickel Oxide that I remove From old Ni MH batteries. I turn it to Nickel Chloride with HCl, then add baking soda to make Nickel Carbonate. Then Nickel Carbonate to Sulfuric acid makes Nickel Sulfate.

y dun u dissolve Ni oxide in H2SO4 directly?

CarlSagans_RayGuns - 11-6-2018 at 07:09

I get really low yields that way, not sure why. It always seems to work better from the carbonate. The Nickel from batteries is also very dirty so the extra step helps clean some of that up.

fusso - 11-6-2018 at 07:43

Quote: Originally posted by CarlSagans_RayGuns

I get really low yields that way, not sure why. It always seems to work better from the carbonate. The Nickel from batteries is also very dirty so the extra step helps clean some of that up.

Had u tried oxalic acid+Ni oxide+H2SO4, like making MnSO4 from MnO2?

NEMO-Chemistry - 11-6-2018 at 15:35

Thank you
Although sulphuric acid is being restricted to 15% in the uk and listed same as Nitric acid, even drain cleaner in areas like mine is getting hard to get. reagent grade price has gone way way up as well. but i will try it.

Shame as i have the nickel metal

OldNubbins - 12-6-2018 at 08:25

The first time I made nickel salts I just electrolysed household vinegar with some nickel 99 welding rods. I fully submerged the anode and just left a cm or so of the cathode in the vinegar. Over a couple of days I was left with a nice dark green nickel acetate solution that I was able to plate from. To speed up the process I would crank up the amps until the solution would get too hot and swap the electrodes to even out the erosion. The watts nickel bath works much better but the acetate solution was functional.

The trinket in the attached image was electroformed over a graphite coated wax form using the watts sulphate bath. My electrodes were baskets of chopped up welding rod zip tied to a graphite gouging rod. It is about 1/2 - 3/4 mm thick and stands up to aggressive polishing. My next step is nickel crucibles.

NEMO-Chemistry - 12-6-2018 at 09:23

thats fab!! acetate i can do i got flakes but got a combustion tube with small hole in bottom of a test tube like thing, so nickel in that and a cathode should do the trick even if slowly. will look up whts bath

Thx
i really love that skull!

NEMO-Chemistry - 15-6-2018 at 08:53

Quote: Originally posted by OldNubbins

The first time I made nickel salts I just electrolysed household vinegar with some nickel 99 welding rods. I fully submerged the anode and just left a cm or so of the cathode in the vinegar. Over a couple of days I was left with a nice dark green nickel acetate solution that I was able to plate from. To speed up the process I would crank up the amps until the solution would get too hot and swap the electrodes to even out the erosion. The watts nickel bath works much better but the acetate solution was functional.

The trinket in the attached image was electroformed over a graphite coated wax form using the watts sulphate bath. My electrodes were baskets of chopped up welding rod zip tied to a graphite gouging rod. It is about 1/2 - 3/4 mm thick and stands up to aggressive polishing. My next step is nickel crucibles.

I have done some looking at this, i can find the wikipedia page on wax with graphite but it dosnt give much detail on how you get the graphite to coat properly. do you have any tips on what kind of graphite and how to do it?

I have played with some simple molds and mainly copper sulphate baths to get the hang of it, i havnt got far though.

A google mainly give me lubricants when i search graphite coated wax moulds.

Any tips would be appreciated. I also have some drain cleaner now so nickel sulphate should be possible with that

NEMO-Chemistry - 15-6-2018 at 11:34

Ok dosnt answer my question but other noobs might like this on Nickel plating. more industrial but interesting

https://www.nickelinstitute.org/~/media/Files/TechnicalLiter...

OldNubbins - 15-6-2018 at 15:44

Quote: Originally posted by NEMO-Chemistry

do you have any tips on what kind of graphite and how to do it?

I use multiple coats (at least 3 or 4, often several more) of hardware store spray lube to build up the graphite layer as much as possible. It is very fine graphite suspended in acetone so it is a balancing act between coats to prevent the solvent from washing away previous layers. If you leave the item for some time, the coating tends to become a bit more resistant to wiping off.

I believe the key to successful plating is starting with a thin copper layer. An alkaline strike (cyanide) would probably be best but I use copper sulfate root killer with a drop of HCl. You have to move the object and have good agitation to avoid dendrite growth and watch closely to make sure the coverage is even. Plating goes slowly over graphite due to the high resistance but I have had decent results with Kohm levels over the surface of the part.

After a thin conductive layer of copper forms, I switch to nickel and build from there. Once there is sufficient nickel for the object to support itself, I remove the mandrel so plating can deposit on both sides. Heating (~40°) and agitation are important for Watts nickel baths.

NEMO-Chemistry - 15-6-2018 at 18:57

One question i get conflicting answers on is about Nickel METAL being carcinogenic or not, i am aware many of the salts are considered so but not sure about the metal. My concern id for making pendents to be worn etc. Anyone actually know if the metal is safe to wear?

OldNubbins - 15-6-2018 at 19:30

Quote: Originally posted by NEMO-Chemistry

One question i get conflicting answers on is about Nickel METAL being carcinogenic or not, i am aware many of the salts are considered so but not sure about the metal. My concern id for making pendents to be worn etc. Anyone actually know if the metal is safe to wear?

If you are not allergic. My wife is allergic to nickel and gets a little rash where the metal contacts her skin.

Diurea - 11-7-2019 at 09:02

I know this is old but I wanted to add something useful I've used for electroplating copper onto things by creating a cupric acetate solution quickly. I would think this would work for nickel too.

Add metal to vinegar and stick in microwave (make sure submerged so no sparks..). The eddy current initiate the ion exchange. Stop before boiling or course. Cool. Go again. If the metal is bubbling its working. Might want to pick up a cheap microwave for experimentation purposes though. Makes your pizza rolls taste funny.. (seriously keep you food and experiments separate)

AJKOER - 14-7-2019 at 05:04

Per Wikipedia on NiCl2 (https://en.wikipedia.org/wiki/Nickel(II)_chloride) to quote:

"In case one needs a pure compound without presence of cobalt, nickel chloride can be obtained cautiously heating hexaamminenickel chloride:[7]

[NiCl2(NH3)6]Cl2 --175 C to 200 C--> NiCl2 + 6 NH3 (g) "

I have prepared the related [CuCl2(NH3)6]X2 by the electrochemical reaction involving add Cu metal to dilute NH3 (aq) in the presence of dilute H2O2 and a touch of sea salt (an electrolyte). Jump start the reaction for a 30 seconds in a microwave (to avoid the characteristic inception period associated with electrochemical reactions). This readily creates with copper an aqueous only product [CuCl2(NH3)6](OH)2 (or related [CuCl2(NH3)(6-x)H2O(x)](OH)2 depending on the concentration of NH3) to which I add MgX2 (I used MgCl2 (aq) to form the target product, which is apparently soluble in ammonia water), and a corresponding precipitate of Mg(OH)2.

[CuCl2(NH3)6](OH)2 (aq) + MgCl2 (aq) = [CuCl2(NH3)6]Cl2 + Mg(OH)2 (s)

And, I would expect the same reaction with nickel metal. Wikipedia (see https://en.wikipedia.org/wiki/Hexaamminenickel_chloride ) notes, with respect to color, to quote:

"Hexaamminenickel is violet, and the copper(II) complex is deep blue"

CAUTION: Not at all certain how safe the above cited prep is for the corresponding nickel salt. Safer path would be the slow unheated path (not microwave assisted). I have a designated old MV for lab prep and would strongly advise not sharing a microwave also employed for food items!

I also suspect I have witness the formation of some [CuCl2(NH3)6]Cl2 as a precipitate in the prep for [CuCl2(NH3)6](OH)2 as an insoluble precipitate as the ammonia concentration falls in the presence of chloride ions. An interesting quote at page 218 in an online ebook, 'Qualitative analysis' by Frederick Pearson Treadwell on using alcohol to form the precipitate, and expect the same for the nickel salt:

"On adding alcohol to the concentrated blue solution, the above compound is precipitated as a blue-violet crystalline substance, which gradually loses ammonia on being heated, leaving behind the cupric salt. "

[Edited on 14-7-2019 by AJKOER]