Nickel Other
DATA SHEET
Satilume® Plus
Issue 11 of 06.06.2001
Replaces issue 10 of 03.05.2001
Contents
Process Information............................................................................................................................. 2
Equipment ........................................................................................................................................... 2
Tanks ............................................................................................................................................... 2
Make-Up.............................................................................................................................................. 3
Working Parameters ............................................................................................................................ 4
Deposition Rates at 55 °C ................................................................................................................... 4
Maintenance ........................................................................................................................................ 6
During Electrolysis .......................................................................................................................... 6
Cleaning and Start of Production .................................................................................................... 7
Application Guidelines .................................................................................................................... 8
Batch-Treatment with Activated Carbon ........................................................................................ 8
Influence of Foreign Organic Substances ....................................................................................... 9
Removal of Pores ............................................................................................................................ 9
Influence and Removal of Foreign Metals ...................................................................................... 9
Recommendations for Wastewater Treatment .................................................................................. 10
Analytical Instruction
Satilume Additive P1 by Titration .................................................................................................... 11
Satilume Plus Carrier P2 by HPLC ................................................................................................... 13
All recommendations and suggestions appearing in these instructions concerning the use of our
products are based upon tests and data believed to be reliable. However, as the actual use of our
products by others is beyond our control, no guarantee, expressed or implied, is made as to the effects
of such use, or the results to be obtained whether the use of our products is made in accordance with
recommendations or suggestions contained in these instruction or otherwise. Furthermore, information
on the use of our products is not to be construed as recommendation to use such products in the
infringement of any patent.
Atotech Deutschland GmbH
Postfach 21 07 80
Erasmusstraße 20 - 24
D-10507 Berlin 21
Telefon (30) 349 85 0
Telefax (30) 349 85 777
Satilume Plus Page 2 / 15
Process Information
 Satilume Plus requires no extra and expensive heating or cooling equipment to operate.
 The Satilume Plus process enables deposition of satin-matt, non reflecting, outstandingly
uniform nickel layers which are insensitive to fingerprints.
 A uniform satin effect can be achieved at layer thicknesses from 10 µm nickel.
 This effect can be individually adjusted by adding Satilume Plus Additive C1 and
Satilume Plus Additive C2. Higher contents result in a matter satin effect.
 Satilume Plus coatings can easily be plated with other metals such as chromium, brass, silver
or gold.
 In order to replenish different evaporation losses the two additives Satilume Plus Additive C1
as well as Satilume Plus Additive C2 are available in different concentrations.
For small evaporation losses we recommend to use the Satilume Plus Additive C2
(4fold concentration)
Equipment
Tanks
For operation of the Satilume Plus nickel bath a special tank (made of mild steel with hard rubber
lining or PVC or PVC-polyester reinforced material) with an an overflow, circulation pump, filter
and separate tank must be used.
Diagram of the Unit
5
5
3
4
5
1
1 = Circulation pump
(membrane piston pump)
2 = Precoat or surface filter with pump
3 =Active tank with overflow compartment
4 = Reserve Tank
5 = Valves
2
5
5
5
5
Satilume Plus Page 3 / 15
Anodes
Rolled pure nickel anodes, electrolytic nickel anodes, or
S-nickel rounds (INCO) in titanium anode baskets.
Anode bags required.
Heating
Heaters made of porcelain, hard glass, or
PTFE heat exchanger made of titanium, graphite.
Mechanical agitation
Mechanical agitation required.
Air agitation must not be used!
Horizontal
Vertical
stroke length
100 mm
60 mm
double stroke/min
20 – 25 (4-5 m/min)
25 – 30 (3-4 m/min)
A 3D mechanical agitation proved beneficial.
Filter must not be used during operation.
(see Cleaning and Start of Production below).
Filtration
Regeneration and maintenance is carried out
with plate filters with cellulose or a
cellulose-activated carbon-mixture.
The filter surface is about 10 cm2 per liter bath volume.
Filtration efficiency of pump: 3 – 4 bath volumes/h.
With mechanical agitation recommended.
Exhaust
Make-Up
Make up of 100 l
Water deionized
Nickel sulfate (NiSO4  6 H2O)
Nickel chloride (NiCl2  6 H2O)
Boric acid
Satilume Additive P1
Satilume Plus Carrier P2
Satilume Plus Additive C1
or alternatively
Satilume Plus Additive C2
Liter
kg
approx. 40
approx. 0.6
approx. 1.5
0.25
47.5
3.8
4.0
0.6
1.5
0.25
0.06
0.06
In all work with Satilume Plus, make sure that all regulations on
operations with caustic substances are carefully observed!
Satilume Plus Page 4 / 15
Working Parameters
Density
1.29 g/cm3 at 20 °C
pH
4.2 (4.0 – 4.4)
During operation the pH slowly increases and must be
checked 1 – 2 times a day. Adjustment downward will
be done with diluted sulfuric acid, chem. pure (5 % by
volume). If too much acid is added, adjust the pH
upward with sodium bicarbonate (10 %).
52 °C (50 – 55 °C)
Temperature
To avoid precipitation, do not allow the plating solution
to cool below 35 °C.
Current Density
4 A/dm2 (3 – 6 A/dm²)
Voltage
Depends on current density, lay out and size of the tank.
The following values apply:
Small and medium sized tanks: 4.0 – 8.0 V
Big tanks : 6.0 – 10.0 V
In case of high bath loading: up to 12.0 V
When titanium anode baskets with nickel rounds are
used the voltage is about 2.0 V higher.
Current efficiency
The cathodic current efficiency is 95 - 98 %.
Deposition Rates at 55 °C
Current Density
A/dm2
3
4 A/dm2
5 A/dm2
Layer Thickness in µm
6 µm
10.0 min
7.5 min
6.0 min
9 µm
15.0 min
11.3 min
9.0 min
12 µm
20.0 min
15.0 min
12.0 min
24 µm
40.0 min
30.0 min
24.0 min
36 µm
48 µm
60.0 min 80.0 min
45.0 min 60.0 min
36.0 min 48.0 min
In most cases, operations at a current density of 4 A/dm2 are possible with a plating solution
temperature of 55 °C. At this the deposition rate is 0.8 µm nickel per minute.
Satilume Plus Page 5 / 15
Make up Procedure
1.
Dissolve the required nickel salts and the boric acid separately in a glass lined steel tank or
a stainless steel tank.
2.
Dissolve the nickel salts in hot and deionized water while adding 0.4 kg/100 l pulverised
activated carbon (low sulfur and iron content, suitable quality can be purchased from
Atotech). For 55.0 kg nickel salts use at least 70 l of water.
3.
Filter the solution into the operating tank and ensure that the solution has a temperature of
between 50 – 60 °C to avoid residues of boric acid in the filter.
4.
Any precipitated boric acid can be dissolved with hot water or hot bath solution. Fill the
plating tank, which contain the anodes, to about 90 % of the required volume and begin
circulation without filtration. Maintain temperature above 50 °C.
5.
The plating solution should be dummy plated with parts for about 2 hours at low current
densities (1 Ah at 1 A/dm2).
Prior to the addition of the required amount of Satilume Additive P1 and
Satilume Plus Carrier P2 check the pH of the plating solution and adjust to
nominal value if necessary.
6.
The nickel content of the Satilume Plus Process should be about 105 g/l.
7.
Afterwards the Satilume Plus Additive C1 or the Satilume Plus Additive C2 will be
added to the bath while stirring thoroughly. Both additives must be sufficiently diluted with
water prior to addition, however at least at a ratio of 1 : 3 for
Satilume Plus Additive C1 and 1 : 10 for Satilume Plus Additive C2.
The additives must never be diluted with plating solution as this will cause precipitation
and can consequently lead to defects in the nickel layers.
8.
After completely filling the tank with the required amount of water mix well for about
15 min.
9.
Switch off pump and allow the plating solution to sit for homogenization for 30 – 45 min.
Afterwards the plating solution will be ready for use. This solution is ready for use for up to
8 hours. Even if not used, this solution must be regenerated and cleaned after about 8 hours.
(see „Cleaning and Start of Production“)
Satilume Plus Page 6 / 15
Maintenance
Concentrations of nickel ions, chloride ions and boric acid can be determined using the usual
methods. Suitable methods of analysis are available on request.
Nickel
Chloride ions
Boric acid
On Make-Up
During Operation
105 g/l
12 g/l
45 g/l
100 – 110 g/l
10 – 20 g/l
45 – 50 g/l
Concentrations of Satilume Additive P1, Satilume Plus Carrier P2 can also be determined
analytically. See attachment.
Satilume Additive P1
Satilume Plus Carrier P2
Satilume Plus Additive C1
Satilume Plus Additive C2 (alternatively)
On Make-Up
During Operation
6 g/l
15 g/l
2.5 g/l
0.6 g/l
5 – 7 g/l
12 – 20 g/l
1.5 – 3.0 g/l
0.35 – 0.75 g/l
Make sure to avoid drag-in of foreign wetting agents from previously used nickel plating
solutions, as they will severely disturb the processing of the Satilume Plus plating solution!
Contaminations which might have been caused by such wetting agents can only be removed
through a treatment with activated carbon.
During Electrolysis
For 10,000 Ah the following is
required:
Satilume Additive P1: 0.5 – 1.0 kg (about 0.5 – 1.0 l)
Satilume Plus Carrier P2: 1 kg (about 1 l)
Satilume Additive P1 and Satilume Plus Carrier P2 will be added to the plating solution where
thorough mixing will be provided. Any water evaporated during operation will be replenished with
distilled, deionized or softened water. Both additives can be mixed with each other.
During operation do not carry out any additions of Satilume Plus Additive C1
and Satilume Plus Additive C2!
Overdosing of the additives must be avoided!
Satilume Plus Page 7 / 15
Cleaning and Start of Production
Independent of the time used, after 8 – 10 hours the satin effect becomes uneven.
For this reason it is imperative to clean the electrolyte after this time frame as follows. It is
recommended to start cleaning immediately after the production stop in order to prevent
precipitation and residues at the tank lining as well as on anode bags:
1. Preparing Filter Pump
Recommended filter mesh size:
For a filter area of 1.0 m2
5 – 10 µm
500 g filter cellulose is needed
additionally.
2. Wash new filter aid onto the filter paper.
3. Filter warm plating solution in the plating tank via overflow for about 4 – 5 hours
(depending on flow rate/capacity of the pumps).
Keep temperature at 35 – 40 °C.
4. Heat the plating solution to working temperature (52 – 55° C).
5. Prior to addition of Satilume Additive P1 and Satilume Plus Carrier P2 the cleaning
performance must be tested in a Hull Cell.
6. Satilume Plus Additive C1 (diluted 1 : 3) as well as Satilume Plus Additive C2 (diluted 1 :
10) will be replenished in the recommended make-up amount. Dilution must never be carried
out using the plating solution! During replenishment avoid local overdosing. Therefore,
additions should be carried out in small quantities while stirring thoroughly. Additions must be
made directly into the working tank and never into the overflow compartment.
7. After addition, the plating solution will be circulated without a filter for about 15 – 30 min. via
the membrane piston pump of the overflow compartment.
8. Switch off circulation pump.
9. Maintain a homogenization phase of at least 30 – 45 min.
10. Afterwards the plating solution is ready to use again.
11. Clean filter unit and remove the used filter cellulose.
12. If, despite following the above mentioned cleaning procedure, the satin effect does not have the
usual appearance, a high-pressure cleaning of the working tank, the anodes and anode bags will
be necessary in order to remove possible residues.
Satilume Plus Page 8 / 15
Application Guidelines
As the additives will be removed partly or totally during the cleaning procedure they need to be
replenished.
The following values apply as guidelines:
After daily filtration with cellulose:
10 - 20 %
5%
100 %
100 %
*
Satilume Plus Carrier P2*
Satilume Additive P1*
Satilume Plus Additive C1 (diluted 1 : 3)* or
Satilume Plus Additive C2 (diluted 1 : 10)*
as % of make up quantities
After every 5 cleaning cycles the plating solution must be cleaned via a celluloseactivated-carbon-mixture!
20 - 30 %
5 - 10 %
100 %
100 %
*
Satilume Plus Carrier P2*
Satilume Additive P1*
Satilume Plus Additive C1 (diluted 1 : 3)* or
Satilume Plus Additive C2 (diluted 1 : 10)*
as % of make up quantities
Batch-Treatment with Activated Carbon
 Dependending on the bath parameters as well as working parameters the plating solution
should be completely cleaned with activated carbon once per month. This treatment helps to
remove residues of reaction products and organic contaminations.
 For this procedure transfer the plating solution to a treatment tank and add 2 – 5 g/l activated
carbon to the plating solution. The temperature of the plating solution must be kept between
40 – 50 °C.
 Remove anode bags from the anodes and wash them with warm water or replace with clean
bags.
 The plating tank must be cleaned with a high-water-pressure cleaner to remove any organic
from the tank walls.
 The filter pump must be provided with new filter paper before transfering the plating solution
back to the working tank.
 After the cleaned plating solution is transfered into the plating tank, the treatment tank and the
filter pump should be cleaned and thoroughly rinsed with water
Satilume Plus Page 9 / 15
Influence of Foreign Organic Substances
To ensure an optimum processing of Satilume Plus the following must be observed:
 Avoid drag-in of foreign organic substances (esp. wetting agent)
 Keep rinsewaters of other plating solutions separate from Satilume Plus as drag-ins have a
negative effect to each process.
 Bright nickel tanks must always be positioned in front of the Satilume Plus tanks.
 Prior to plating with Satilume Plus a thorough activation of the surface is necessary. It is
recommended to use fluoride containing activations for nickel plating and micro-etching for
copper plating. Suitable Atotech products are available.
Removal of Pores
If hydrogen pores evolve on the bottom of the parts the boric acid content can be increased to about
50 g/l. It is also possible that pores occur due to improper dilution of the Satilume Plus
Additive C1 or C2. Using a combination with the Satilume Plus Stabilizer can prevent the
formation of pores in these cases.
Influence and Removal of Foreign Metals
Contaminations of foreign metals, especially copper and zinc, will produce dark Satilume Plus
deposits.
To remove possibly existing foreign metals the plating solution needs to be dummy plated with a
big cathode area (corrugated iron) and current densities from 0.05 – 0.2 A/dm².
Satilume Plus Page 10 / 15
Recommendations for Wastewater Treatment
Rinse water
Nickel can be precipitated by adjusting the rinse water pH to between 9.5 – 10 with NaOH. The
filtered solution can subsequently be sent to final neutralization.
Concentrated Operating Solutions
The following options are possible when concentrated nickel solutions must be treated.
When nickel is to be recycled, it is generaly necessary to treat these nickel solutions separately
from other solutions. The following recycling methods are typical, although others can be
recommended:
 Electrowinning of nickel using an appropiate electrolytic cell.
 Treatment of nickel concentrate, or of a precipitated nickel sludge, by a specialized recycling
company. If these methods are not possible, the nickel concentrate can be treated by adjusting
the pH to between 9.5 - 10. This should be done only with water that is free of complexing or
chelating agents. To achieve good settling of the precipitated metal hydroxides, add the
concentrated solution to rinse waters in the treatment plant at a maximum concentration
of 20 % before pH adjustment takes place. Floccuation aids may also be required.
IMPORTANT NOTE : Be sure to observe all local regulations concerning the limit values of
pollutants including the general regulations on dangerous materials!
Satilume Plus Page 11 / 15
ANALYTICAL INSTRUCTION
Satilume Additive P1
by Titration
Issue2 of 18.02.2000
Replaces issue 1 of 21.01.2000
Reagent required*
 KBr/KBrO3 solution 0.05 M
 Potassium iodide solution 0.1 M
 Hydrochloric acid conc.
 Starch solution
 Sodium thiosulfate volumetric solution 0.1 M
Procedure




Fill 50 ml sample** into a 250 ml iodine flask. Add
20.0 ml KBr/KBrO3 solution and
20.0 ml HCl conc. Cover the solution and allow to react in the dark for
20 min. Then add
Satilume Plus Page 12 / 15
 20.0 ml potassium iodide solution and
 1 ml starch solution and immediately titrate with
 0.1 M sodium thiosulfate volumetric solution until the colour changes to green.
(a blank value is determined with DI water until the colour of the solution changes from black
to green)
Example
During titration of 50 ml nickel bath, 7.6 ml/l 0.1 M sodium thiosulfate volumetric solution was
used.
Calculation
(20.0 – 7.6)  0.48 = 6.0 ml/l Satilume Additive P1
IMPORTANT NOTE : Be sure to observe all local regulations concerning the limiting values
of pollutants including the general regulations on hazardous materials!
*
**
Unless otherwise stated, these are always analytical grade substances.
Volumes given exact to a decimal point must be measured with a volumetric pipette.
Satilume Plus Page 13 / 15
ANALYTICAL INSTRUCTIONS
Satilume Plus Carrier P2 by HPLC
Issue 2 of 20.09.2000
Replaces Issue 1 of 20.01.2000
Principle of Method
RP-HPLC
Pumps
Type
WATERS 510 or equivalent type
Mobile phase
Methanol / Water (20 / 80) + 1 ml/l H3PO4
Rate of flow
1.0 ml/min
Pressure
2000 PSI
Injection System
Type
WATERS WISP 712 B or normal injection valve
Injection volume
50 µl
Summing time
10 min
Satilume Plus Page 14 / 15
Pre Column
Material
HYPERSIL ODS
Granulation
5 µm
Length
5 cm
Inner diameter
4.6 mm
Column
Material
HYPERSIL ODS
Granulation
5 µm
Length
25 cm
Inner diameter
4.6 mm
Detector
Detection
UV-Detector
Type
WATERS 481 Lambda Max or equivalent type
Wave length
198 nm
Aufs.
1
Response
0.1
Internal Temperature
25 °C
Procedure
Preparation of the Samples
 1.00 ml sample is pipetted into a 1,000 ml volumetric flask and filled to the required volume
with DI water.
Satilume Plus Page 15 / 15
Measurement
For external calibration standards with 10.0 ml/l and 25.0 ml/l Satilume Plus Carrier P2 are used.
These will be diluted 1 : 1000 (analogous to the sample) and injected directly.
The measure peak level of the sample should be within the peak level of the standards.
Calculation
The content in the sample of Satilume Plus Carrier P2 is determined via external
calibration.
Evaluation is carried out via the software
Accuracy of the method
RSD of the method
Retention time:
±5%
about 5.4 min