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Nickel General Operating Instructions

This document provides general operating instructions for Atotech nickel plating processes. It discusses equipment requirements like approved tank materials, preparation of new tanks, and storage/purification tanks. It also covers pumps, fittings, heating, filtration, agitation methods, electrical equipment, and solution preparation. The key recommendations are to use approved synthetic-lined steel tanks, ensure equipment compatibility with nickel solutions, provide adequate filtration and agitation, and consult Atotech for specific system design details.

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0% found this document useful (0 votes)
330 views

Nickel General Operating Instructions

This document provides general operating instructions for Atotech nickel plating processes. It discusses equipment requirements like approved tank materials, preparation of new tanks, and storage/purification tanks. It also covers pumps, fittings, heating, filtration, agitation methods, electrical equipment, and solution preparation. The key recommendations are to use approved synthetic-lined steel tanks, ensure equipment compatibility with nickel solutions, provide adequate filtration and agitation, and consult Atotech for specific system design details.

Uploaded by

Nicole fralix
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 14

Sheet No.

: GOI-Nickel
Revision: 04/30/04T-107
IMDS ID No.: Not Relevant

Technical Information
General Operating Instructions
For Atotech Nickel Plating Processes
EQUIPMENT

Plating Tanks

Rubber or synthetic-lined steel, composition, ceramic or glass tanks, which have been approved for use with
Atotech nickel processes, should be used. Lead-lined, stainless steel, wood or pitch-lined plating tanks are not
approved. Contact your local Atotech representative for information on approved tank linings.

The following procedure should be used to prepare a newly lined plating tank for use with Atotech nickel
processes:

1. Rinse the tank thoroughly with water to remove dust and other loose foreign matter.

2. Hand scrub tank with a mixture of three parts by volume of water to one part by volume of the Atotech
anti-pitter used. This will facilitate the removal of oil and grease.

3. Rinse with water.

4. Fill the tank with a water solution containing 2% by vol. (20 ml/l) of hydrochloric acid and 0.2% by vol. (2
ml/l) of Atotech anti-pitter.

5. Heat the solution to 120-140o F (49-60o C), stirring occasionally. Associated equipment should be
cleaned by circulating the above solution throughout the entire system. Maintain these conditions for
approximately 8 to 12 hours, or until ready to use the tank to hold the nickel plating solution.

6. Empty the tank and rinse well. The tank is now ready for use with Atotech nickel processes.

Important Notice Regarding the Attached Information:


The statements, technical information and recommendations contained in this document are based on tests and data that are believed to be reliable. Further, as the actual use of
our products by others is beyond our control, no guarantee of any kind is made as to the effects of such use, or the results to be obtained, whether the use is made in accordance
with the recommendations or suggestions contained herein or otherwise. This document is not contractual and NOTHING HEREIN CONSTITUTES A REPRESENTATION OR
WARRANTY THAT THE GOODS DESCRIBED ARE FIT FOR A PARTICULAR PURPOSE OF A CUSTOMER or that their use does not conflict with any existing patent rights. The
exclusive source of any warranty and of any other customer rights whatsoever is on the Atotech invoice. Also, since this data sheet may be provided by electronic media, Atotech
cannot guarantee the accuracy or originality hereof. Any alterations made to this document other than by Atotech corporate headquarters is expressly prohibited.

Atotech USA Inc. 1750 Overview Drive, Rock Hill, SC 29730


Telephone: 803-817-3500 • Fax: 803-817-3666
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 2

The plating tank jacket should be thoroughly insulated from electrical grounds and stray currents through wet
flooring, water pipes, or any other source. The plating tank should be located in an area where the solution will
not be contaminated by lint, dust or grit from buffing and polishing operations, or other manufacturing
processes.

Storage Tank

A storage tank is necessary for make-up, treatment, purification, or storage of the plating solution. The tank is
preferably lined with a suitable synthetic lining. A lead lining should only be used if the NiCl 2 • 6 H2O content of
the nickel plating solution is below 8 oz /gal (60 g/l). The thin protective crust that forms on the lead surface
should not be disturbed in order to prevent contamination of the solution with lead as a result of plating solution
attack on exposed clean lead surfaces. If a rubber or synthetic lining is used, it must be approved for use with
Atotech nickel processes. A suitable heating coil of sufficient size to raise the solution to a temperature of 150-
170o F (66-77o C) should be provided. It is suggested that the coil be placed on the side of the tank to permit
unhampered cleaning of the tank after use. A small sump or a sloping bottom has proven helpful in emptying
the storage tank with a minimum of solution loss.

Electrolytic Purification Tank

In some cases, notably in plating zinc base die-castings, the solution is being contaminated continuously with
metallic impurities. When such contamination is troublesome, continuous or intermittent, electrolysis can be
used to purify the solution without interrupting the plating operation. This requires a suitably lined small cell,
equipped with a series of anode and cathode surfaces, operated at 2-5 amps per square foot (0.2-0.5 amps
per square decimeter), and provided with a pump to maintain constant circulation of the plating solution to and
from the plating tank. Details of the tank size, current requirements, etc., can be obtained from your local
Atotech representative.

Pumps and Fittings

Construction materials of pumps, fittings, circulation lines and all associated equipment such as filters and heat
exchangers should be approved for use with Atotech nickel plating processes. Where nickel solutions contain
8-10 oz /gal (60-75 g/l) or more of NiCl 2 • 6 H2O, special precaution should be taken to ensure that the
equipment is compatible and will withstand the added corrosiveness of the plating solution. Consultation with
the vendor of the equipment and/or Atotech is suggested.

Heating

Glass-coated steel, Duriron or Karbate steam coils, electrical heating units, and other suitable types as well as
external heat exchangers may be used for heating the plating solution. Lead and titanium heating coils can
satisfactorily be used in many instances. The proper selection and installation of the heating equipment is of
utmost importance. In planning a new installation, it is advisable to consult with your local Atotech
representative. Also, please refer to the section in this bulletin on "Pumps and Fittings".

Filtration

For mechanically agitated baths, the plating solution should be circulated through a filter at a rate sufficient to
turn the tank volume over at least once every two hours. Similarly, air-agitated solutions should be turned over
at least once per hour. The filter may be of any type that will keep the solution free from suspended dirt or
foreign particles.
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 3

Return lines should be of non-metallic materials, or if they are metallic, they should be suitably lined to prevent
any bipolar condition in the electrical circuit. They should be positioned in the tank so that direct impingement
of the solution stream on the work is avoided. Circulating lines must be arranged so that a recirculating slurry
feed tank can be used.

No solution should be returned directly to the plating tank after an addition to the filter without first determining
by recirculation that the solution is perfectly clear. The slurry tank used for this purpose must be placed above
the level of the pump.

Mechanical Agitation

Solution agitation is strongly recommended. Slow oscillatory movement (e.g. 3-8 ft. per min.) is sufficient in still
tank operation. Ordinary chain speeds in automatic plating operations are usually satisfactory.

Air Agitation

A low-pressure blower having sufficient capacity to provide filtered, oil-free air should be used. "Compressed"
air should definitely not be used. The blower should be large enough to provide air at a pressure of one pound
per square inch for each 18 inches of solution depth, and a volume capacity of one cubic foot per minute for
each linear foot of immersed, perforated pipe. If the blower is mounted below the level of the plating solution,
an anti-siphon device should be installed at the uppermost portion of the header pipes. All immersed pipe
should be fabricated from suitable synthetics approved for use with Atotech nickel plating processes. Metallic
pipe, in any form, is not approved. Specific details concerning the design and installation of air agitation
systems can be obtained from Atotech.

Solution composition requirements may vary according to the type and degree of agitation. Consult with your
local Atotech representative for more information.

Bus Bars and Other Electrical Equipment

The electrical equipment (e.g. bus bars, anode and cathode contact hooks, plating racks) should be
constructed to carry an ample uninterrupted flow of current up to a reasonable load greater than the highest
current densities anticipated. In general, current loads on copper bus bars should be designed for 750 amps
per square inch of cross-sectional area. Loads in excess of 1,000 amps per square inch will result in
overheating and high voltage drops. Bus bars, as well as anode and cathode hooks, must be kept clean at all
times to ensure good electrical contact. When cleaning bus bars, precautions should be taken to prevent
copper and dirt, which might be loosened during cleaning, from falling into the plating solution. Anode hooks
and bus bars should be protected against accumulation of salts caused by splashing or dripping of electrolyte
during the removal of work from the plating tank. This accumulation might otherwise cause roughness of the
deposit by crumbling and falling into the solution, as well as insulating the anode hook.
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 4

SOLUTION PREPARATION

A storage tank should be used to prepare a new Atotech nickel plating solution. The storage tank, if newly lined
with rubber or synthetic materials, should be first leached with a solution containing 2% by vol. (20 ml/l) of
hydrochloric acid and 0.2% by vol. (2 ml/l) of non-pitter. The solution should be heated to 120-150o F (49-66 o
C) and maintained at that temperature for at least eight hours with occasional stirring. The tank should then be
emptied and rinsed thoroughly before use. Please refer to the "Plating Tanks" section for more details. The
plating solution may be prepared as follows:

1. Fill the storage tank two-thirds full with clean water and heat to 140-160o F (60-71o C).

2. While mixing, add and dissolve the required amount of nickel sulfate.

3. While mixing, add and dissolve the required amount of nickel chloride.

4. After all of the nickel salts have dissolved, add enough nickel carbonate to raise the pH to at least 5.2.
Stir thoroughly.

5. Add 2 lbs/100 gals (2.4 g/l) of Atotech Activated Powdered Carbon and stir for 30-60 minutes.

6. Allow the solution to settle for 3-4 hours or, preferably, overnight.

7. Filter the treated solution into a clean plating tank.

8. While mixing, add and dissolve the required amount of boric acid.

9. Dilute to final volume with water and heat to operating temperature.

10. Adjust the pH to 3.5 with well-diluted sulfuric acid.

11. At this point, it is advisable to "dummy" the solution by electrolyzing at about 5 amps per square foot
(0.5 amps per square decimeter) for 12 hours. Use of agitation and filtration during this period is
recommended.

12. After the electrolysis period, readjust the pH, if necessary.

13. Add the required amounts of addition agents.

14. Circulate the solution through a filter for twenty minutes and commence plating.
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 5

SOLUTION MAINTENANCE AND CONTROL

Nickel Sulfate

The nickel content should be determined at least once a week and adjusted at regular intervals. Normally, a
concentration of 30-60 oz/gal (225-450 g/l) of nickel sulfate is required, since this range provides a sufficiently
high metal concentration for all purposes. If the plating job is particularly difficult (e.g., deep recesses, sharp
corners, irregular shapes, etc.) or if the current concentration required is above 1.5 amperes per gallon (0.4
amps per liter), the nickel salts concentration should be maintained at the high end of the suggested range.

Nickel Chloride

The nickel chloride content should be determined and maintained within the limits specified at the same
frequency as that suggested for nickel sulfate. The use of Atotech nickel chloride is recommended for this
purpose. Low nickel chloride concentrations can result in poor anode corrosion and low efficiency leading to
depletion of the nickel content of the solution and/or breakdown of the addition agents. Please refer to the
section on "Anode Area".

Boric Acid

The boric acid content of the plating solution should be determined and adjusted at least twice a week. Its
concentration should be maintained within the specified limits for the following reasons:

1. It is important that the upper concentration limit of boric acid not be exceeded. When the boric acid
concentration reaches about 7 oz/per gallon (52.5 g/l), crystallization takes place when the solution is
allowed to cool. This can causes roughness of the deposit.

2. While boric acid is not generally recognized as an efficient buffer in the pH range used for nickel
plating, it is an experimental fact that there is noticeably less gassing at the cathode and increased
operating efficiency when the boric acid content is kept within the specified limits. Excessive gassing at
the cathode can cause streaking, gas pocketing, and is an indication of low operating efficiency.

3. Low boric acid levels can also contribute to an "orange peel" type of pitting.

Anode Area and Anode Current Density

The importance of maintaining full anode area cannot be over emphasized. Active anode area, i.e. that area
subject to electrolytic corrosion, must be maintained at the highest practical level. In "still" tanks, sufficient
active anode area must be provided to maintain the anode current density below 18 amps per square foot (1.9
amps per square decimeter). In highly agitated tanks, e.g. air-agitated, the anode current density should not
exceed 30 Amps/sq.ft. However, the type of nickel anode material and anode bag material as well as agitation
can raise or lower these arbitrary anode current density limits. If the limiting current density is continually
exceeded, there will be a tendency for the anodes to polarize leading to loss of current, possible loss of deposit
ductility and poor corrosion protection.

Anode area should be checked frequently and anode material added to provide the maximum area. Anode
hooks must be kept clean and shielded to prevent poor contact with anode bus bars and roughness due to
nickel salts falling back into the plating tank.
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 6

OPERATING PRECAUTIONS

Anode Bags

The use of anode bags, specially treated for complete removal of sizing and lubricants, is essential for good
results. Conventional rolled or cast anodes should have bags fitted several inches longer than the anodes and
should be tied around the anode at the base of the hook so that this extra length is left at the bottom of the
anode to contain anode sludge. Anode basket bags should be approximately one inch larger in each cross-
sectional dimension and, preferably, no more than two inches longer at the bottom.

With air-agitated solutions, care must be taken to prevent "flapping" at the bottom of the anode bags.
Conventional rolled or cast anodes should have weights placed at the bottom of the bags. These weights
should be constructed of an inert material such as a smoothly rack-coated nickel anode section, glass or
ceramic.

Because of the weight of the anodes and the relatively sharp edges of the baskets at their ends, special care
must be taken when placing bags over the anodes. Bagged anodes should never be placed on top of one
another, as this will invariably cut or bruise the bags. Bags should be examined frequently for tears, cuts or
damage, and replaced where necessary, since fine particles from the anodes will cause severe deposit
roughness if allowed to enter the solution. The use of two bags or double walled bags may be advisable in
installations where frequent cutting or tearing occurs.

General Precautions

1. Prevent work from falling into the plating tank.

2. Remove any fallen work as soon as possible before its dissolution can contribute to solution
contamination.

3. Prevent racks from becoming built-up with nickel to the point where particles become detached.

4. Prevent damage to the tank linings and make prompt repair when such damage accidentally occurs.

5. Observe and report all unusual phenomena such as excess gassing, changes in appearance of the
deposit, etc., so that the causes may be determined and conditions quickly corrected.

6. Maintain firm and solid rack contact with the parts to be plated. There should be no appreciable drop in
voltage through rack contacts.

7. Prevent damage to rack coatings and make immediate repairs should such occur.

8. Bus bars and racks should have sufficient cross-sectional area to provide adequate current carrying
capacity. Usually, about one square inch of copper bus bar should be provided for each 750 amperes
expected at maximum load.

9. Bipolar conditions must be avoided, as the effects from this are very harmful.

10. Air introduced into the solution through faulty pumps and filters can be very harmful. Excessive air in
the solution will develop foam-type pitting, black burn and "orange peel". Good pump maintenance and
installation of water seals on the pump are recommended to avoid trouble from this source.
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 7

EFFECTS OF IMPURITIES

General

Poor nickel deposits are very often caused by impurities that have been introduced into the plating bath. In
most cases, such difficulties can be avoided or minimized by employing good plating procedures such as:

1. Thoroughly cleaning the work before plating to remove buffing compounds, greases, oils, oxide film,
etc.

2. Using clean acid dips, properly maintained cleaning solutions and adequate running water between
each operation to minimize drag-in.

3. Preventing grease and oil used on the tank mechanisms from falling into the nickel solution.

4. Preventing work from falling into the plating tank. Remove fallen work as quickly as possible before
dissolution can contribute to solution contamination.

5. Where degreasers are used, carefully check ing the work prior to entering the plating tank to ensure
that the cleaning cycle has removed buffing compound abrasive, etc., from irregularly shaped work.

6. Taking precautions to prevent degreaser fluid from setting into the nickel solution.

Impurities in a nickel plating solutions fall into three major classifications: 1) suspended or solid matter; 2)
organic matter consisting of soluble and colloidal organic contaminants; and 3) any soluble metal or its anion.

METALLIC IMPURITIES

While the limits for impurities given below represent maximum tolerances, maintaining the least possible
concentration is consistent with good plating practices.

Zinc

Zinc present in nickel plating solutions will become critical at concentrations of approximately 100 ppm (0.1 g/l).
However, in many cases, depending on operating conditions and the combined effects of other impurities, the
effects of zinc may be noted at much lower levels. The effects usually include black streaks, grayness in
recessed areas, brittleness and reduced corrosion resistance of the deposit.

The zinc concentration should be kept as low as possible. For methods of removal, see "Solution Purification-
Zinc".

Chromium

Chromium is a particularly detrimental impurity in any nickel bath. Amounts in excess of 10 ppm (0.01 g/l) as
hexavalent chromium are harmful, causing loss of efficiency, loss of throwing power, peeling and brittleness.
For removal of chromium impurities, see "Solution Purification-Chromium".
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 8

Iron

The presence of iron may cause dullness in recessed areas, poor corrosion resistance, pitting and roughness.
The iron content should be kept under 150 ppm (0.15 g/l), or lower should conditions dictate. For removal of
iron, see "Solution Purification-Iron".

Copper

Copper contamination will cause grayness in recesses, loss of color, brittleness of deposit, and rough edges.
The copper content of the bath should not exceed 20 ppm (0.02 g/l) for best results. For removal of copper,
see "Solution Purification-Copper".

Ammonia

The presence of more than 1500 ppm (1.5 g/l) of ammonia may cause deposit brittleness and increased
hardness. Ammonium compounds should never be used to increase the pH of Atotech nickel plating solutions.
Ammonium compounds cannot be removed by treatment.

REMOVAL OF METALLIC IMPURITIES

Zinc

Zinc contamination can be removed by either low current density [2-5 amps per square foot (0.2-0.5 amps per
square decimeter)] electrolysis (dummying) or high pH treatment using nickel carbonate. Where zinc
contamination is a problem, continuous removal is advised by the use of an electrolytic purification tank (see
“Equipment"). In less severe instances, intermittent low current density electrolysis using "dummy" cathodes
(preferably of the corrugated type) is advised. In very severe cases, batch treatment of the solution will be
necessary as directed under "Solution Purification-High pH Treatment with Nickel Carbonate".

Chromium

In most cases, chromium in operating nickel solutions is present in the trivalent state. Therefore, the chromium
is usually removed by high pH treatment with nickel carbonate procedure described under "Solution
Purification". In cases where contamination is definitely attributed to hexavalent chromium, it will be necessary
to reduce the chromium with sodium bisulfite or sodium thiosulfate. Consult with your local Atotech
representative when reducing agents are to be added since excesses can be detrimental to the nickel deposit.

Iron

Ferric iron maybe removed by a high pH treatment as discussed under "High pH Treatment". Ferrous iron can
also be removed by a high pH treatment (above pH 5.3), but it is sometimes difficult to obtain this high pH. In
these cases, the iron must be oxidized to the ferric state. Consult with your local Atotech representative when
oxidizing treatments are to be performed.

Copper

Electrolytic purification by dummying the solution at 2-5 amps per square foot (0.2-0.5 amps per square
decimeter) is widely used for the removal of copper. During dummying, the pH should not be allowed to exceed
3.5. Please refer to the "Equipment-Electrolytic Purification Tank" section.
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 9

ORGANIC IMPURITIES

The type and number of organic contaminants is beyond the scope of this outline. In general, organic
contamination is introduced into the nickel solution from carryover of prior processing solutions, leaching of
associated nickel plating equipment or air currents around the plating tank.

Examples of contaminants that can enter the nickel plating solution by carry over include caked buffing
compound, stamping or machinery oils, drawing compounds, cleaning solutions, and additives in prior
processing solutions. Contaminants that enter because of leaching include improperly cured tank linings and
patches, inadequate de-sized anode bags, poor rack coatings, improper filter aids, etc. Examples of airborne
contaminants are equipment lubricants, buffing lint and compounds.

The effects of organic contamination vary. They can range from loss of deposit ductility, poor color, poor
leveling, pitting, roughness and staining. The effects on the process include a loss of efficiency, loss of
throwing power and increased consumption of addition agents.

Most organic contaminants can be removed by treatment with activated carbon. In some cases, oxidation
treatments are necessary prior to treatment with activated carbon. Organic contaminants that cannot be
removed by the treatments mentioned under "Solution Purification" may permanently harm the solution, thus
the importance of preventing these contaminants cannot be over-emphasized.

If organic contamination is indicated, laboratory tests using the procedures given under "Solution Purification"
should be performed.

SOLUTION PURIFICATION

The purification of nickel plating solutions to remove detrimental foreign substances may be divided into four
general categories:

1. Filtration through a "filter aid” material to remove insoluble matter

2. Chemical treatment with nickel carbonate followed by filtration to remove inorganic impurities such as
iron, zinc, copper chromium, aluminum, silica, etc.

3. Chemical absorption onto activated carbon to remove organic impurities such as grease, oils,
decomposition products, etc.

4. Electrolytic treatment to remove metallic contaminants such as copper, zinc and lead.

Filtration

While the selection of the filter unit is a matter of choice, the filter and its auxiliary equipment should be lined
with a material that has been approved for use with Atotech nickel plating processes. The recommendations of
the filter manufacturer should be followed in selecting the size and type of filter.
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 10

Carbon Treatment

The following procedure should be used for the removal of contamination caused by oils, greases, buffing
compounds and other organic impurities:

1. Transfer the plating solution to a clean and suitably lined storage tank.

2. Adjust the pH of the solution to any point between 3.0 and 3.5.

3. Adjust the temperature of the solution to 150-170o F (66-77o C).

4. Add four to eight pounds of Atotech Activated Powdered Carbon per 100 gallons (4.8-9.6 g/l) of plating
solution. Four or five pounds (4.8-6.0 g/l) of carbon are usually sufficient, but, in cases of badly
contaminated solution, eight pounds 9.6 g/l) or even more may be necessary. Two separate carbon
treatments using 4 lbs per 100 gallons (4.8 g/l) are usually more effective than one treatment using 8
lbs per 100 gallons (9.6 g/l). However, two filtration steps are involved.

5. While maintaining the temperature, stir in the carbon carefully for at least two hours or more. Allow the
solution to settle for an hour or more. Clean plating tank and anode bags; replace worn out bags and
anodes.

6. Filter the purified nickel solution back into the cleaned plating tank using a filter pre-coated with a filter-
aid type material. While filtering, draw the solution from the top to avoid picking up loose quantities of
carbon that might restrict the solution flow or even stop it entirely.

7. When filtering the carbon-bearing solution, it is advisable to also add about one pound of "filter aid" per
100 gallons (1.2 g/l) of plating solution. This should be added slowly to the storage tank near the
suction hose as the level of the solution is reduced.

8. Adjust solution level to final volume and adjust the pH to within range. The pH can be increased by
circulating the solution through a filter unit that has been packed with nickel carbonate on "filter aid", or
lowered by the addition of diluted sulfuric acid. For further data on the use of nickel carbonate, please
refer to the section "High pH Treatment with Nickel Carbonate".

9. Adjust addition agent(s) levels, as required.

10. Resume plating operations.

High pH Treatment with Nickel Carbonate

Where a high pH is required for the removal of metallic impurities, the following procedure should be followed:

1. Transfer the plating solution to a clean and suitably lined storage tank.

2. Adjust the temperature to 150-170o F (66-77o C).

3. Prepare a slurry of nickel carbonate and water by adding eight pounds (960 g/l) of dry nickel carbonate
to one gallon of water containing 0.25 fl. oz. (2 ml/l) of anti-pitter is added. Stir this mixture, preferably
with a mechanical stirrer, until completely dispersed. Do not add dry nickel carbonate powder directly to
the plating solution in the storage tank; always use a slurry.
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 11

4. With constant stirring, slowly add the nickel carbonate slurry to the heated solution. The amount of
nickel carbonate to be added will vary depending on the original pH of the solution, but an amount
equivalent to five pounds of dry nickel carbonate per 100 gallons (6 g/l) of plating solution is usually
sufficient.

5. While maintaining the temperature, stir solution for one hour or more. Then, check the pH of the
solution and adjust again with nickel carbonate slurry until the pH is at least 5.2.

6. Allow the solution to settle for at least eight hours or, preferably, overnight. Clean plating tank and
anode bags; replace worn-out bags and anodes.

7. Filter the treated solution back into the cleaned plating tank using a pre-coated filter. While filtering,
draw the solution from the top to avoid restricting the flow or even stopping the filter entirely.

8. When filtering, it is advisable to assist in maintaining an even rate of flow by adding about one pound of
"filter aid" per hundred gallons of plating solution. This should be added slowly to the storage tank near
the suction hose, as the level of the solution is lowered.

9. Reduce the pH to within the operating range using diluted sulfuric acid.

10. It is important to follow the procedure outlines in the "Filtering Precaution" section.

Combination Treatment with Carbon and Nickel Carbonate

Treatments involving both activated carbon and nickel carbonate are ideally performed separately and in the
order given. Lacking sufficient time to perform both treatments, a satisfactory compromise can be used where
the solution is first treated with activated carbon followed by nickel carbonate. The following procedure should
be used:

1 - 5. Perform Steps 1 through 5, as directed under "Carbon Treatment".

6 - 13. Instead of allowing the solution to settle as per Step 5 above, perform Steps 3 through 10, as
directed under "High pH Treatment".

14 - 16. Complete Steps 9 through 11 under "Carbon Treatment".

Oxidation Treatments

The following treatments should be used only on advice of Atotech. All precautions should be observed
carefully to ensure that oxidizing materials are not present in the treated plating solution.
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 12

Treatment with Hydrogen Peroxide and Carbon

1. Pack the filter with about 2 lbs. per 100 gallons (2.4 g/l) of Atotech Activated Powdered Carbon.
Transfer the solution to the treatment tank by pumping through a packed filter. This is done to remove
part of the anti-pitter.

2. Allow the solution to cool to 100-110o F (38-43o C) and adjust the pH to 3.5.

3. With agitation, add one quart per 100 gallons (2.5 ml/l) of 30% Hydrogen Peroxide (100 volume).

4. With agitation, agitate the solution and maintain the temperature at 100-110o F (38-43o C) for at least
two hours.

5. Raise the temperature to 160o F (71o C) and maintain it for two hours to drive-off excess peroxide.

6. Add 4-6 pounds per 100 gallons (4.8-7.2 g/l) of Atotech Activated Powdered Carbon and agitate for at
least two hours at a temperature of 150-160o F (71o C).

7. Allow the solution to settle thoroughly, meanwhile, clean plating tank and anode bags. Replace worn-
out bags and anodes.

8. Filter the treated solution back into the clean plating tank.

8. Add the required amounts of addition agent(s), check and adjust pH, if necessary, and resume plating
operations.

Combination Treatment-High pH, Peroxide and Carbon

Follow the step-by-step procedure numbered 1 through 6, as outlined above under "Treatment with Peroxide
and Carbon", and then continue as follows:

7 - 14. Follow Steps 3 through 10, as directed under "High pH Treatment".

15 - 17. Complete Steps 9 through 11 under "Carbon Treatment".

Special Precautions for Peroxide and Carbon Purification of Nickel Solutions

The following points allow the operator to perform a treatment with a greater degree of effectiveness and
reduce the possibilities of an unsatisfactory deposit due to improper purification of the solution.

1. Step 1 is considered essential and failure to perform this part of the treatment may lead to incomplete
removal of impurities.

2. The conditions specified under Step 2 are important and should be followed as closely as possible. The
low temperature is required to prevent decomposition of the hydrogen peroxide until it has served its
oxidizing function. For the same reason, a pH of 3.5 is best. A low pH makes it difficult to remove the
peroxide under Step 5, and too high a pH increases the decomposition rate of the peroxide.
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 13

3. The complete removal of hydrogen peroxide under Steps 5 and 6 is of utmost importance. Failure to
remove the peroxide completely will cause subsequent plating problems due to the action of any
residual peroxide on the addition agents. To ensure complete removal, the temperature should be
maintained at 160o F (71o C) until a test shows the absence of hydrogen peroxide.

Test for the Presence of Peroxide in Nickel Plating Solutions

1. Dissolve 5 grams of Potassium Iodide in 100 ml water. Add 5 grams of soluble starch and heat until the
starch is completely dissolved.

2. Place one drop of the plating solution onto a filter paper.

3. Place two drops of the iodide-starch indicator over the solution spot on the filter paper.

4. Observe the color. If a blue color develops within 5 seconds, peroxide is present.

General Information on the Peroxide Test

Copper interferes at concentrations of 10 ppm (0.01 g/l), however, the reaction at these concentrations is slow
and no color will develop in 5 seconds. Most nickel baths contain less copper than this amount. The starch -
iodide reagent is not stable, but will last about a week depending on storage conditions. It is suggested that the
reagent be prepared fresh, as needed.

Oxidation with Permanganate

This treatment will remove many organics that activated carbon alone or peroxide-carbon treatments will not.
Generally, a solution of potassium permanganate is added, followed by a carbon and high pH treatment. The
amount of potassium permanganate to be used will vary with the degree of contamination and should be
determined by the Atotech Customer Service Laboratory. The following treatment procedure should be used:

1. Transfer plating solution to a clean, suitably lined storage tank.

2. Adjust the pH of the solution to between 3.0 and 3.5.

3. Adjust the temperature of the solution to 150-170o F (66-77o C).

4. Dissolve the required amount of potassium permanganate in an appropriate amount of water (usually
about one pound of permanganate to one-half to one gallon of warm water) and add slowly to the
plating solution while stirring. Continue agitation for two hours.

5. Continue as directed under "Combination Treatment with Carbon and Nickel Carbonate". Due to the
large volume of insoluble material that is filtered out, it is frequently easier to perform two filtration
steps, i.e., the first treatment with carbon and then with nickel carbonate.
GENERAL OPERATING INSTRUCTIONS-NICKEL PAGE 14

WASTE DISPOSAL

This material must be disposed of in accordance with all applicable federal, state, and local regulations and
permits. Consult the MSDS for additional regulatory information. The information contained herein is general in
nature and may not apply to each application.

GENERAL SAFETY PRECAUTIONS

When working with this product(s), ensure that all health, environmental, and safety regulations and standards
are met. Avoid direct contact with this material. Do not inhale associated mist, vapors, and/or dust. Maintain
and limit exposure as recommended by OSHA, ACGIH, and other state and local regulations. Wash
contaminated clothing before reuse. Always comply with the Hazard Communication Standard, 29 CFR
1910.1200. Emergency showers and eyewashes must be readily available.

It is recommended that the plating chemistry product(s) referred to in this Technical Information Sheet be used:
(a) in accordance with the information provided in product specific MSDS; and (b) in compliance with all
applicable requirements and guidelines established by OSHA, NIOSH, ACGIH, NFPA, and others.

NOTE: A Material Safety Data Sheet (MSDS) for this product(s) is available upon request from Atotech USA
Inc., Customer Service/Sales Support Group, 1750 Overview Drive, Rock Hill, SC 29730.

REVIEW MSDS BEFORE USING THIS PLATING CHEMISTRY AND FOR SPECIFIC INFORMATION. A
precautionary approach should be used when there is potential for chemical exposure -- this includes
minimizing exposure potential, rapid decontamination, and medical follow-up.

TELEPHONE NUMBERS

General Information: (803) 817-3500

To Place an Order: 1-800-PLATING

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