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@szbalogh  Yes, that would have been nice to have the composition. Obviously, he runs a factory and therefor buys the fluids in bulk.

All I can read from the bottle that it's a base and it is called Nickel-Neutral 023-001-003-010 and the supplier is HPE GmbH.

Do you happen to have the composition of the activation-fluid?

Edited by Endeavor
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3 hours ago, Endeavor said:

@szbalogh  Yes, that would have been nice to have the composition. Obviously, he runs a factory and therefor buys the fluids in bulk.

All I can read from the bottle that it's a base and it is called Nickel-Neutral 023-001-003-010 and the supplier is HPE GmbH.

Do you happen to have the composition of the activation-fluid?

 Thank You! I just needed the right keyword. 

http://www.google.com/patents/US3417005

 

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@szbalogh It seems that you found it :) and that you are at home in chemistry. When reading this patent, I understand till it gets to the chemical-compositions........ I can tell you exactly how to drill a 5km vertical & horizontal hole in the earth for gas/oil, but chemistry is way above my head. Once you figured it out, maybe you could be so kind to translate the names and amounts needed (like I did in a post on page 2 of this thread) for the more mortals like me?

Also, I'm very keen to get the composition of the activator-fluid. As far as I'm aware, not so much chemicals are needed (I think HCl is one) and could be done by the less chemistry orientated ;)  It would be very nice if you could give me a hand with that one !?

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4 hours ago, Endeavor said:

 

The neutal nickel bath seems easy to prepare. Have some Ni-sulfate made from nickel coin dissolved in sulfuric-acid. Citrate is a citric-acid You can buy in every grocery. Ammonia solution from a household shop. Gluconic acid is the only missing part it is also called E574 food additive. I will get that somewhere. Making their sodium salt is easy with lye or more convenient with baking soda. Should be no problem but a lot of time getting all ingredients in clean solid form to be able to measure them according the patent.

As for the activator. If i have time, i will make some tests with screws and nuts.

Here are my test on a non prepared zinc-coated screws. The one on the right is dipped in copper-sulfate, the others in my miracle liquid from baking powder :)

 

20160422_084722.jpeg

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Seems you are doing very well :thumbsu:

Once you get the required results, it would be nice if you could make a list with chemicals required and the quantities, say per liter......(or in US gallon). Being an European, I prefer Liters :) Perhaps also, where the chemicals can be obtained or in which household product(s) they are "hiding".

Citric acid is E330, a food additive which I obtained from a DIY wine-making store. Among other uses, it's used to increase the acidity of wine. It's also used in some beers, like nettle-beer ;)

Sulfuric acid from a car-battery or in some drain-unblocker products.

Sodium Salt is that not normal Sodium Chloride (NaCl), normal kitchen salt?

Gluconic acid was, according to Wikipedia, initially distilled from urine (hence the name) and as you said, it's used as an food-additive E574........I always thought some foods tasted suspicious! No idea yet where to get it, and no, I'm not going that route......... :D

Anyway, you are doing great and hopefully we can come up with a whole range of plating fluids which can be home made!

We have already the cleaning fluid and electrolyte for brush plating. Missing is the activator (which shouldn't be too hard given the receipt) and all the metal-fluids. It would be fantastic if we could work that out :jig:

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NaCl (table salt or simply salt) wont change the pH. Its from strong base and strong acid. Baking soda is from strong base and weak acid and if mixed with a stronger acid (compared to bicarbonate) it will form salt (sodium-cirtate for example) and CO2 and H2O.

I think that gluconate and citrate are buffers and used to maintain pH. Maybe we can leave the gluconate out and use just more citrate.

The patent suggesting another surface preparation method like anodic cleaning, dipping in acid salt solution and finally dipping in triethanol amine solution. But they say "conventional methods were not particularly good for this bath", which i think will be sufficient for us :) so i will stick to the sulfuric acid cleaning first.

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Wow, really fantastic result @Endeavor!

The ground work you've laid here is going to come in quite handy for me in the future too as I'm usually working on vintage pieces and have been considering a complete restoration including replating.  Thanks for sharing!

 

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@RyMoeller I hope the information here will benefit you as well ;) There is more to come and hopefully forum member Szbalogh can help us out with some more DIY plating fluids.

Depending on the donor-materials I get from forum member Ramrod, my plan was to make a walkthrough about watch-hands, watch-cases, main-plate & bridges and the crown itself. Submerged plating seems to be the most effective with good results, but it needs more complicated (expensive) fluids. Since I now finally received some pure-copper and pure-nickel, I like to try brush-plating as well (only suitable for small parts which can be totally covered by the sponge). The composition for the easy brush-plating electrolyte is further back in this thread. Lacking is the composition of the activator fluid.........

All exciting stuff.......:jig:

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Ordered yesterday some Ni strips from China (usually i get my stuff from there for very cheap:) ). Till then started making NiCl from the remaining nickel coins submerged in the mixture of hydrochloric acid 50 mL (grocery 5-15%, more concentrated is faster) and hydrogen peroxide (35% from hairdressers shop) 20-30 mL. The solution was left outside overnight (~5 Celsius) and has nice  green color now and the half of the coins are gone. It may be much faster with filed down Ni powder. I will get out the pieces and file them down.

Ususally industry needs mirror finish right after the plating. They simply cant polish every piece. But for us and for 1-2 pieces... There is no need for complications for nickel plating on brass and copper. Simple NiCl solution is adequate. The surface will be semi-bright or matte but You can polish after. Tried it on some custom watch hands. 

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@szbalogh  Sounds very good....... and I like the fact that even a hairdresser is a source for chemicals :biggrin::thumbsu:

The Nickel fluids I have are of industrial standard, and the results are as you can see on the bracelet, without additional polishing. If the end results are semi-bright or matte, polishing may become a problem when the objects are highly fragile like watch-hand or if the objects are uneven / recessed, like main-plates, bridges, perhaps the wheels etc. It would be nice if we can get the fluids to such a level that the "after-work" gets reduced to a minimum or none.

Besides, the plated layer is already very thin, so there is a risk of going "through-it" while polishing.......

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Played a bit yesterday with my electroless copper on zinc plating solution.

The piece is a see-through caseback from a chinese watch. Sanded down to shiny appearance. Left from the piece is degreasing liquid (benzin), top left is the plating solution and finally demineralized water.

20160428_213103.jpeg

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I had to move it in the solution continuously or it got grey. I got a nice red copper layer finally:

20160428_214256.jpeg

The layer seems hard enough (for being copper), i couldt scratch it down with my nails. However, it is really thin, 10.000 grit diamond powder made through it if polished to long and with big force. An electrolytic plating is necessary afterwards and before the nickel layer. Next time i will prepare the electrolytic copper and nickel baths and try make the platings on this layer.

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@szbalogh You are doing some nice tinkering and making progress ;)

Maybe I like to throw in some thoughts; You are using benzin as de-greaser. To my mind, benzin still contains some grease. The solution I used was normal tap-water with 10% caustic soda and a few droplets of liquid soap. The object is then cleaned using electricity as you would with plating (described earlier in this thread) and thereafter rinsed in demineralized water. That seems much cheaper, less hazardous and no toxic fumes......  ?

The copper-layer I produced with brush-plating, wasn't very thick either, but that was due to the contact time between the sponge and the object (also described earlier)

Curious about your next steps...... :thumbsu:

 

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My old nickel sulfate batch finally recrystallized. Made an electrolytic nickel bath quickly. 1.5g NiSO4, 0.25g boric acid and a pinch of p-toluen sulfonic acid in 10mL water.

The zinc ring (electroless copper striked) was washed down with a tissue soaked in banzynum. Two AA batteries parallel were used az a power source. Plating was carried out at ~70 Celsius.

Here is how it looks like after the bath rinsed in water:

2016-05-01 15.13.46_1920.jpg

And after rubbing with 10000 grit polishing paste by hand:

2016-05-01 15.17.59_1920 fényes.jpg

Now i can go for the watch case and the cromium bath preparation. 

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I'm impressed, also with the chemicals you are using...... (the latter; you lost me completely.....)

Just like the Swedish cook in the muppets, but the end result seems to taste well...... :)

 

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  • 3 weeks later...

Per Endeavor's request, I'm jotting down the method I used to strip the chrome down to the brass from my Vostok Komandirskie's case bezel and crown. This can't be done on Amphibia cases, as they are made of stainless steel. 

Very easy process:

  • Remove the movement from the case and take off the bezel
  • Remove the gasket from the crown and the wire from the bezel.
  • Soak the case (ok to leave the crystal), the bezel (enamel will be ok), and the crown in hydrochloric acid. 10%-20% strength will suffice.
    • I used muriatic acid, which I got at the hardware store. This was already diluted to 32% HCl, I diluted this further with 50/50 and it was fine for stripping
  • The reaction will begin immediately and it will act fast, so keep your eyes on it and remove the pieces as soon as they look good. (Took mine 10 min total to strip).

Your mileage may vary. Googling 'stripping vostok hydrochloric acid' will bring up a bunch of posts and videos. 

I must add: PLEASE be careful with the HC: the fumes are terrible for you, it can burn your skin, it can damage surfaces. Wear gloves, do in a well ventilated room HANDLE WITH EXTREME CARE!!!!

Let me know if you have any questions.

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