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Nickel pitting




2007

I have a problem with a bright nickel bath :

nickel metal 70 gr/lt
nickel chloride 65 gr/lt
boric acid 45 gr/lt
saccarine 5 gr/lt
allyl-sulphonate 8 ml/lt
PPS 70-90 ppm
propargil alcohol 5-10 ppm
pH 4,5
temperature 60°C
surface tension 30 dyne/cm
cathodic current density 4 amp/dm2

- it's not a cleaning problem
- it's not a substrate problem
- we have this problem on the flat surfaces
- we use a double anodic cover and a 2 micron filtration system (20 turn over/hour)
- we use Venturi system
- we haven't iron or other metallic contamination
- the problem increase with a stronger agitation of the solution
- random distribution at all current density

please help me!

Fabio Crolli
finishing shop - Firenze, Italia



2007

I don't see any wetter in your formulation.
You should use a wetter which serves as an anti-pit.

sara michaeli
sara michaeli signature
Sara Michaeli
Tel-Aviv-Yafo, Israel



First of two simultaneous responses --

24 dyne/cm will work better.

jeffrey holmes
Jeffrey Holmes, CEF
Spartanburg, South Carolina
2007



Second of two simultaneous responses -- 2007

Are you using any wetting agent? Also, I note that you are filtering at 20 turn overs per hour - I would consider this very high and only to be used in special circumstances. This high turn-over, coupled with the use of venturi, could cause your problems, especially if the dulling is associated with the venturi. When the electrolyte is moving too fast, the effects of additives such as brighteners are nullified. Try reducing the filtration rate to about 8-10 per hour and moving the venturi to an area where they do not impact on the workpiece

trevor crichton
Trevor Crichton
R&D practical scientist
Chesham, Bucks, UK



2007

Thank you all
we use a classic wetting agent to reduce the surface tension to 30 dine/cm
we tried to reduce it to 24 and we had no results.

Fabio Crolli
- Firenze, Italy



2007

Thank you Trevor
decreasing the Venturi agitation the bath works better but we need more brightener (PPS + propargyl alcohol) to obtain the same leveling effect so, by our experience Venturi increase the leveling effect
I agree with you that the problem is too much liquid movement but only STOPPING the Venturi I have no pitting and so I lose the Venturi benefits
we work on fashion accessories and we need mirror plating
so the question is :
can I use Venturi without having pitting
sorry for my English
regards,

Fabio Crolli
- Firenze, Italy


How about seal leaking and ultra small air bubbles are pumped into the solution. I have never seen it, but there are literally hundreds of people that have had this problem.

James Watts
- Navarre, Florida
2007



My favorite brightener for nickel is sodium saccharin - it takes only about 0.5-1.0 g/l to give a good brightness and it hardens the nickel as well. However I see that you also use saccharin, so it may be worth asking your supply house for a better brightener. You can also use butyne diol or coumarin.

trevor crichton
Trevor Crichton
R&D practical scientist
Chesham, Bucks, UK
2007



2007

I use much more saccarine (3-5 gr/lt) and I add propargil alcohol (or butyne-diol) + PPS because I need a strong leveling. This is a standard range of brighteners in our application field. I have not the leveling I need with your formulation.
Have you got any other ideas ?
Thank you

Fabio Crolli
- Firenze, Italy



2007

Pitting is most related to Filtration because the Pump is install outside the Plating tank.
The Pipe leaks air in and get mixed in the Pump .
Test: Get a 600 to 1000 ccm beaker [beakers on eBay or Amazon], collect the Solution from the Tank and hold Quick!
Against bright light .
If any Air is mixed, the solution is like milky and take 10 to 30 seconds to clean
Into a clear Bath solution
If not milky, any fine Air going up like Champagne is a sign.

Joseph Liekmeier
- Paderborn, Germany


Yes, I checked pump filtration system and I'm sure that there isn't fine air in the solution (obviously not milky while working).

Fabio Crolli
- Firenze, Italy
2007



Lower your bath temperature to 55-58 degree C.
hydrolysis would happen to nickel if temperature too high.

John Hu
- Singapore
2007



First of two simultaneous responses -- 2007

John,
I agree that if the temperature of a sulphamate bath is too high,it will hydrolyse and cause stress problems, but this normally only happens at 70 °C, so holding it at 60 °C will be OK. Indeed I have run sulphamate baths at 60 °C for many years without any stress problems.

trevor crichton
Trevor Crichton
R&D practical scientist
Chesham, Bucks, UK



Second of two simultaneous responses --

I tried to take the temperature down to 58 - 55 - 50 degrease but the pitting was the same.

Fabio Crolli
- Firenze, Italy
2007



First of two simultaneous responses --

I agree with Trevor and I want clarify that I'm using a sulphate (not sulphamate) bright nickel
Do you think I can solve my problem using sulphamate ?

Fabio Crolli
- Firenze, Italy
2007



Second of two simultaneous responses --

Fabio,
What type of wetting agent are you using?
For Venturi you must use a wetter which is adequate to a mechanical agitation and not a wetter used for air agitation!

sara michaeli
sara michaeli signature
Sara Michaeli
Tel-Aviv-Yafo, Israel
2007



I know you originally said that most of the more common causes of your problem have been eliminated, but the most common causes of pitting are: no or insufficient wetting agent; wrong pH, too little agitation; too much agitation, bath contamination, surface contamination, dust or other debris in the tank. As a long shot - check to see if your anodes are Ok; they may be producing sludge that is getting into the bath and then onto the plating surface and causing pitting. Otherwise, go back and re-check all the process parameters and the condition of the tank. What happens if you do a Hull cell test on the bath - if it still pits, it is the solution; if it doesn't - it is the process. If all else fails, you may need to dump the bath and start again, after cleaning out the tank.

trevor crichton
Trevor Crichton
R&D practical scientist
Chesham, Bucks, UK
2007



Fabio,
We use what appears to be essentially the same bath chemistry and have the same issues from time to time. What we have found is this:

Make sure the acids in the pre-plate cycle are fresh and changed out on a regular basis, try dumping the your acids and see if this lessens the pitting problem.

The other issue may be contamination from breakdowns of the PA and the PPS these would tend to "plate out" the more violent the agitation.

The other issue is dependent on how often you add back your secondary brightener component. If you add back say 1000 mLs every 1000 amp/hours cut this down into smaller more frequent adds of 100 mls every 100 amp/hours for example. This keeps a good amount of PA in the bath at all times which is what will really give you a nice leveled deposit.

I would still do at least a heavy carbon treat (test out in the lab?) remembering that PPS breakdowns are very hard to remove.

J. Ott
plating shop - Hbg, Pennsylvania
2007



Fabio Crolli
Do you say what the problem is only in flat surface in concave part do you have the same problem, because I have the same problem additional to this some areas it have distortion of the nickel film.

Jose G Cordova
Personal - Mexico
2007



Jose Cordova,
If you are routinely running an electroforming bath, you must have a good book and perhaps take a course in electroforming. There are several ways to control stress in a sulfamate bath (this is the main reason to use it). Temperature, amperage and pH variations all move the stress curve. You can literally tailor your part to zero stress. Get a recent copy of the Metal Finishing Handbook or any of the "must have" books suggested here.

Guillermo Marrufo
Monterrey, NL, Mexico
2007


In the process of electroforming using Nickel Sulfamate, somebody know the methodology to the determine the concentration of the boric acid in the solution ?

Jose G Cordova
- Tijuana, Mexico
2007



Jose, the simplest way to analyse for boric acid is to take 10 mls of the nickel plating solution and dilute it with DI water to 100 mls. Take 20 mls of the diluted solution and put it into a 300ml conical flask; add 5-10 mls of mixed indicator (which is made from 1g bromocresol purple [affil links] mixed with 0.5g bromothymol blue in 100 mls ethanol). If the solution turns yellow, titrate it against N/10 sodium hydroxide to a blue end point. If the solution is blue, titrate it against N/10 hydrochloric acid to a yellow end point. The colour of the indicator is pH dependent, so the starting colour will depend on the bath's pH. Then add 1.5 mannitol and the solution will turn yellow. Titrate this yellow solution against N/10 sodium hydroxide to a blue end point. The amount of boric acid can be calculated as:
mls N/10 NaOH X 3.1 = gm/l boric acid

The end point can be difficult to determine, so I have often diluted the original solution by a factor of 2, so the titration is done against 5 mls of bath diluted to 100 mls. The exact end point is also quite difficult to get, so I would recommend you practise it with known concentrations of boric acid and see just when you get the end point. I also recommend you shake the solution for about 45 seconds to make sure it doesn't revert back to yellow.

I have only limited experience of using 1,4-butyne diol as a leveler in a nickel bath, but I believe when it decomposes it does not form harmful by-products - this is one of its advantages. However, I do see you are using 65g/l NiCl2. This is almost certainly the cause of your stress. The problem with nickel sulphate baths is that you need the presence of a halide to promote anodic dissolution of the nickel. Most people use chloride as it is cheap and cheerful. However, it will induce tensile stress. You have two options; firstly replace the NiCl2 with NiBr2, or secondly, convert you system to nickel sulphamate. The beauty of nickel sulphamate is that you do not need chloride present if you use sulfur nickel rounds as the anode. Hence you do not get stress. This will also allow you to reduce the amount of saccharin you put in your bath. If you really insist on using chloride, then reduce it to 40g/l and it MAY solve your problem. My personal option would be to use sulphamate; - it may cost a bit more, but it will give you better quality plating and in the long run will save you money by reducing your scrap rate.

trevor crichton
Trevor Crichton
R&D practical scientist
Chesham, Bucks, UK
2007


On the electroforming of Nickel the part it have deformation this is an effect of stress. I will like to know how reduce the stress in the plating this produce a distortion of the image.

Jose G Cordova
Personal - Mexico
2007



October 26, 2010

I have a problem with a bright nickel bath: Cloudy-hazy deposition

nickel metal 70 gr/lt
nickel chloride 60 gr/lt
boric acid 45 gr/lt
saccarine 5 gr/lt
sodium allyl-sulphonate 7 ml/lt
1,4-butyne diol 40-60 ppm
propargyl alcohol 5-10 ppm

Ph 4,5
temperature 60
cathodic current density 3 amp/dm2

- it's not a cleaning problem
- it's not a substrate problem
- we use Venturi system
- we haven't iron or other metallic contamination

please help me!

Osman TURAN
- Izmir, TURKEY



Check your bath analysis and tell us what it is, not what it should be. I suspect the bath brighteners are out of balance.
You don't say what type of bath it is, but if it is sulphamate, I would drop the pH to 3.6-4.2 - it won't solve your problem, but it may help in the overall running.

Trevor Crichton
- Chesham UK
October 28, 2010



Hazy nickel deposit, I think high brightener or leveling component in brightener is too high. Run hull cell panel
"as is"then dummy the hull cell panel then run the regular
panel.

popat patel
Popatbhai B. Patel
electroplating consultant - Roseville, Michigan
October 29, 2010




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