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Design and construction of electroplating


apparatus for cyanide less silver on
copper plating

NSF Extreme Ultraviolet Engineering Research Center, Colorado State University

Yu-ping Shao, Advisor: Jorge Rocca
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Table of Contents

Abstract ......................... 4
Introduction
Electroplating background ......................... 4
Target device description ......................... 5
Device challenges ......................... 5
Summary of previous work ......................... 6
Project management ......................... 6
Implementation .........................
Experimental setup ......................... 6
Solution level ......................... 7
Apparatus features ......................... 9
Tank construction ......................... 9
Deposition rate ......................... 10
Procedure .........................
Precleaning ......................... 12
Surface preparation ......................... 13
Plating ......................... 13
Operating steps ......................... 13
Soak clean ......................... 14
Electrolytic Clean ......................... 16
Deoxidizing phase ......................... 18
Plating ......................... 20
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Conclusion ......................... 24
Future work recommendation ......................... 24
Appendix
List of figures and tables ......................... 25
Percentage volume information ......................... 25
Chemical formula and symbol ......................... 26
Original vendor summary ......................... 27
Supplier tank design ......................... 29
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Abstract
The electroplating of silver on copper is currently performed by an external shop;
therefore, little control is exerted over properties pertaining to electroplating such as thickness,
surface quality, and purity. Therefore, by building a device with controlled electroplating
capability. We can assure that deposition thick goes up to 15m, has a uniform surface finish and
controlled deposition rate. The device should be capable of depositing 10 to 15m of pure silver
on the experiment copper target device.

Introduction


Deposition of silver through electrochemistry


Figure 1: Electroplating tank diagram

Electrodeposition of silver is done through the use of an external electron supply. The
cathode of the setup, in this case the copper target device, and the anode of the setup, in this case
the silver are connected to their perspective ends. The external power supply drives the process
when silver surface is ionized to form cations that are then deposited upon the copper surface.

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Target Device:






















Figure 2: a) Target device. b) Target device dimensions.


The actual target device is made of copper and has parts of the surface removed so that
strips of approximately 2mm in width can be seen spiraling along the surface from top to bottom.
10 strips are found on the surface with each about 1mm spaced from another.
The target device undergoes electroplating through which the silver deposited on the
strips is from 10 to 15 m in thickness. In a high vacuum environment, a EUV laser source
causes the ablation of silver.

Device challenge
Generally, electroplating is performed within a chemically and electrically non-reactive
tank with electrolytic solutions to cause the transfer of ions from anode to cathode. While
electroplating copper unto nickel is almost spontaneous and can be performed with immersion
electroplating, deposition of silver on copper is not. This is due to the ranking of materials in
their electron affinity. The ranking: gold, silver, copper, nickel, shows that copper requires a
striking agent in addition to the electrolytic solution. Industrial electroplating of silver unto
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copper in 95% of the electroplating shops requires the use of potassium ferrocyanide. Since
ferrocyanide is a highly hazardous material due to high toxicity, an alternative of non-cyanide
plating is adapted. The solution instead contains organosilver complexed with thiosulphate ions

Project management
This is a single effort. The student is responsible for all the phases of the project except
fundraising, which is provided by the CSU Extreme Ultraviolet Engineering Research Center.

Summary of previous work
With 95% of all plating shops adopt a cyanide containing process, effort to conduct
electroplating in a small scale is not well attempted. The primary enabler for this project is based
upon recent work by EPI Chemicals, from which a electronic class, cyanide less chemicals have
been formulated to be used in industrial application.
Main work will be to synthesize the information given by the vendor technical data, and
plating tank norms used by the plating shops. For both the consideration of space and
application, barrel plating and equipment pertaining to barrel plating is investigated.

Implementation

Experimental setup
Due to corrosive vapor produced during the pre-cleaning stage, the entire device must be
kept within a fume hood. In addition, ACS certified respirator must be worn during the plating
procedure to reduce the risk of breathing in corrosive material.
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Figure 3: Layout of the setup.

The motor is running at 6RPM when supplied with 12V. The electrodes involved in the
plating and electrolytic cleaning require another power source. In this case, Agilent 6632A
power supply is chosen for its high stable voltage capability while running on constant current
mode. In addition, its programmable capability offers a degree of control with proper software
interface.

Solution level

A 4 liter beaker has the height of approximately 9.34. In designing the apparatus, the
positioning of components must fit within component constraints. When filled up to 3L, the
solution level is approximately 7. The chemicals ordered from the supplier are enough to make
3L in the volume of chemicals. Therefore, the shaft that is attached to the cathode and the
extenders that hold the silver anode must extend deep enough to be fully submerged within the
solution. In addition, to eliminate fringe effects on the coating surface, 1.5 is left for extra space
between the surfaces of the cathode to the surface of the anode bars.




8





































Figure 4: Illustrating solution level.
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The Apparatus Features
1. Temperature and chemical resistant tank
2. Rotating target mounting shaft
3. Height adjustable cover
Tank construction:
Due to the rational discussed above in the precleaning procedure, uniform electric fields
distribution is achieved by using a cylindrical tank. Pyrex glass is chosen as the tank material for
reasons pertaining to being chemically and electrically unreactive, and able to withstand high
temperature.

Corrosion
resistant
Electrically
unreactive
Size (8
DIA)
High
temp.
Machinability Cost
Stainless steel Yes Wont
affect
plating
process
Yes Yes
(might get
hot)
Difficult High
Glass Pyrex
(borosilicate)
Yes Yes N/A Yes N/A
(specialized
glassblowing)
Med.
Plastic
Acetal
Yes Yes Yes No Good Med.
Plastic
Polycarbonate
Yes Yes Yes Yes Good High
Plastic -
Polyethylene
Yes Yes Yes No (melts
at 180F
Good Low
Table 1: Materials considered for tank


Since Pyrex glass is not machinable, it is essential to find a glass apparatus in laboratory
ware catalog with the desired dimensions. A beaker with the capacity of 2000mL has 130 x
190mm for height and outer diameter respectively.
A motorized rotator is mounted on the armature and a threaded shaft attaches the motor
output shaft to the cathode sharing the same axial line. Rotating the work piece at the rate of 6
RPM distributes the deposition evenly on the cathode target device. Given 9 in the shaft length,
the height of the tank provides enough head space from the top of the solution to the bottom of
the lid with 2.5 in. in between.
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Adjustable back for cover height becomes necessary to operate the device within the
fume hood. Since beakers are of different sizes, especially between the ones that kept the plating
solution, and the ones for cold water rinsing. Adjustable cover makes it easier to operate.

Deposition rate:

The rate of deposition is a function dependent upon the metal-solution interface, the
kinetics of the deposition, the nucleation and growth process of the metal lattice and the structure
and properties of the deposits. A good estimation of the deposition rate is as followed

q Na n m Q * * * = 1.1

Q total deposition cathodic charge

m number of gram moles of metal deposited

n number of e
-
in the reaction

Na Avogadros number

q fundamental charge of electron

F - Faradays constant

By definition

q Na F * = 1.2

Given that

1 23
10 022 . 6

= mol N
A


C q
19
10 602 . 1

=

mol
C
. F 44 96473 =
F n
Q
m
*
= 1.3

dt I Q

= 1.4

dt
F n
I
m

=
*
1.5
11

V
w
D = 1.6

D density

m Mw w * = 1.7

Mw molecular weight

A area

T - thickness
T A
w
D
*
= 1.8

dt
D A F n
I
Mw
D A
w
T

= =
* * * *
1.9

Now assume that current is held constant.

D A F n
t I Mw
T
* * *
* *
= 1.10


Mw(silver) = 107.8682 amu

D(silver) = 10490
3
m
kg


Oxidation state(silver) = +1

Ag
+1
+ e
-
Ag

so n = 1


) 10 49 . 10 ( * * ) 44 . 96473 ( * ) 1 (
* * ) 8682 . 107 (
3

=
A
t I
T

A
t I
T
* * 10 07 . 1
7

= 1.11

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From the supplier specs, the optimal cathode current density (
A
I
) is 1 to 3
2
ft
A
or 1.07 x 10
-7
to
3.22 x 10
-7

2
m
A



For thickness of 16 m and running at 1
2
ft
A


) 10 03 . 1 ( * ) 10 07 . 1 (
) 10 16 (
7 7
6

= t

t = 1.30*10^8 4.36*10^7sec -> 1.5 to 0.5day


Procedure

The entire plating flow can be summarized in four steps.

1. Precleaning
2. Surface preparation
3. Plating
4. Post-cleaning/ polishing
Precleaning
The precleaning process combines both soak cleaning and electrolytic cleaning. For soak
cleaning, the device to be cleaned is immersed under a solution diluted with a mixture of surface
agents, detergents, and suspension agents. While in electrolytic cleaning, the process removes
smut, soil deposits, and prepares the surface for plating. The apparatus used in electrolytic
cleaning should bear similarity to the one used in plating. The process of cleaning achieves the
best result based on the uniform distribution of electric field lines from the anode to the cathode
surface. The quality of the cleaning predicts the success of good electroplating.
Electrolytic cleaning is performed after soak cleaning. The process may cause mild
oxidation on the copper surface visible as darkening spots. These are removed using acidic salts
before the actual plating.

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Surface preparation
Before plating, the work surface must be activated by immersion in a solution created
from a dry, acidic salt that etches and temporality deoxidizes the copper surface allowing for
greater time for the plating process

Plating
The conventional method of electroplating involves the use of potassium cyanide as a
striking agent, and potassium carbonate as electrolytic solution. The plating solution provided by
the supplier electroplates silver directly onto copper without a striking agent. The elimination of
cyanide reduced cost of waste management. The solution also works in room temperature and is
specified by the supplier to have exceptional covering and throwing power, and produces fine-
grained, smooth, dense, hard deposition layer with low porosity and high luster.
The concentrated liquid must be diluted with deionized water. The solution must operates
within the pH scale of 8.8 to 9.5 and should be adjusted accordingly using KOH or nitric acid.
Keeping the pH below 10 and temperature between 120F is essential in keeping the
effectiveness of the bath.
A ratio of 2 to 1 should be kept between the surface area of pure silver anode to the
copper cathode. While a filtration device using carbon filter is recommended, air agitation alone
provided by aquarium air tank is sufficient due to the small-scale nature.
The best way to run the electroplating apparatus is to divide the operation into several
stages. Before running the machine, titration chemicals for each of the solution tank involved
must be prepared in advance to ensure the flow of the operation without interruption in between.
Running each stage is now organized into lab format to convey the clearest understanding from
the suppliers specifications.

Operating steps
For the actual plating procedure, the procedural steps have been further subdivided into
various stages. Organized as a collection of labs, the manual is meant to convey operational
knowledge as well as calculation as quickly as possible.
Included with each step is also the method of testing involved, as well as pre-quantified
amount of solution chemical mixture used for testing
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1. Soak cleaning
2. Electrolytic cleaning
3. Cold water rinse
4. Deoxidizing phase
5. Cold water rinse
6. Plating
7. D.I water rinse
8. Dry

Soak Clean

Vendor Operating parameters:
Electrolytic cleaning Soak cleaning
Concentration: 4 to 10 oz/gal. of water 8-16 oz/gal of water
Temperature: 140 to 200F 140 - 200F

Immersion time: 15 seconds to 2 minutes (
zinc and copper)
1 to 5 minutes (steel)
5 10 minutes
Polarity: Anodic (reverse current) N/A
Current Density: 10 to 30 amps. (zinc and
copper)
50 to 100 amps. (steel
N/A
Table 2: Soak clean vendor specs.

Recommended parameters
Bath concentration 8 oz/gal

Bath charge-up

Equipment
125 mL Erlenmeyer flask
25 mL pipet
Clean 2.5 L beaker
Hot plate
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WARNING: Operate within a fume hood and wear a respirator!

Material is caustic soda
and the vapor produced by heating the solution can cause burn. DO NOT MIX E-Kleen
with acidic material or other chemicals.

Material
E-Kleen pellets

Procedure
1. Fill beaker with water.
2. Heat up the temperature of the beaker content to hot enough (~120 F) to melt the E-Kleen
pellets.
3. Measure out E-Kleen pellets in weight (~180 g).
4. Add the pellets slowly to the warm water to avoid sputtering.
5. Stir the solution with pellets until completely dissolved.

Calculation
1 L = 0.264 gal
1 oz = 28.349 g

Note: Need to fill up to 3 L of E-Kleen solution. This is to make sure that the electrodes will be
completely immersed in a 4 L beaker.

3 (L) x 0.264 (gal/L) x 8 (oz/gal) x 28.349 (gram/oz) = 179.62 g
Testing the bath

Equipment
Clean 1 L beaker
25 mL pipet

Material
-Methyl orange indicator
-1 N HCl
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Procedure
In an overview, the method described takes a sample of the bath solution, and titrate it with 1 N
HCl. Based on the volume of the HCl (in mL), concentration can be calculated.

1. Allow the solution to cool to room temperature.
2. Take a sample of the solution from the bath using a 25 mL pipet. Transfer to a clean 125
mL Erlenmeyer flask.
3. Add 25 mL of water.
4. Use Methyl orange indicator to produce a yellow colored solution. Add 5 drops. For
strips, hold the strip with a tong.
5. Titrate with 1 N HCl until the indicator turns orange-pink.

Calculation
Concentration of E-Kleen (oz/gal) = (mL of HCL) x (0.3125) x (Normality of HCL)
In this case given that normality is 1 N.
Concentration of E-Kleen (oz/gal) = (ml of HCL) x (0.3125)
Concentration should be 8oz/gal

Running soak cleaning
Equipment
Hot plate
Thermometer

1. Heat up the solution to 160 F on the heat plate.
2. Soak the cathode into the solution for 10 minutes

Electrolytic clean
Vendor Operating parameters:
Electrolytic cleaning Soak cleaning
Concentration: 4 to 10 oz/gal. of water 8-16 oz/gal of water
Temperature: 140 to 200F 140 - 200F

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Immersion time: 15 seconds to 2 minutes (
zinc and copper)
1 to 5 minutes (steel)
5 10 minutes
Polarity: Anodic (reverse current) N/A
Current Density: 10 to 30 amps. (zinc and
copper)
50 to 100 amps. (steel
N/A
Table 3: Electrolytic clean vendor specs.

Bath charge-up
If steps for charging the soak clean bath have been followed, the used bath can also be used for
electrolytic cleaning

Running the cleaning step

Equipment
DC power supply
Hot plate
Thermometer

Procedure
10 ASF has been selected for copper cleaning

1. Attach the steel anode bars onto the lid of the device.
2. Heat the solution to 160 F.
3. Immerse both the cathode and the steel anodes.
4. Connect the positive terminal to cathode, and negative terminal to anode. This effectively
reverses the current flow for anodic cleaning.
5. Turn on the supply, select current mode and limit it to 0.86 amps. (For detail of the
calculation, refer to running the plating step)
6. Let it run for 2 minutes.
Cold water rinse
Equipment
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1 L beaker

Procedure
1. Fill the 1 L beaker up to 0.8 L.
2. Submerge the cathode within the cold water for 5 minutes.
3. While rinsing the cathode. Take off the steel bar electrodes.
4. Wash the other electrodes.

Deoxidizing phase

Vendor Operating parameters:
Range Optimum Temperature Time
8-24 oz/gal 16 oz/gallon 65-90F 2-5 minutes
immersion
Table 4: Surface activation vendor specs.

Recommended parameters
Concentration: 16 oz/gal ratio
Temperature: 90 F
Time: 5 minutes immersion

Bath charge-up
Equipment
1 L beaker
WARNING: MUST wear respirator and wear gloves. Material is corrosive.

Material
E-Pik pellets
D.I. water

Procedure
1. Fill the 1 L beaker up to 1 L of D.I. water.
2. Measure out E-Pik pellets. ~ 120 gram.
3. Add salt slowly to the D.I. water
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4. Stir until the pellets completely dissolve.

Calculation
Fill up the beaker completely to ensure full immersion of the target copper electrode.
1 L x 16 (oz/gal) x 0.264 (gal/L) x 28.349 (g/oz) = 119.7 g

Testing the bath
Equipment
1 L beaker
Pipet

Material
50% Sulfuric acid (H2SO4)
KI/EDTA solution
D.I. water
0.1 N Sodium thiosulfate
Starch indicator

Procedure
1. Take 2 mL of the bath sample.
2. Add 3 mL of 50% sulfuric acid.
3. Add 50 mL of D.I. water.
4. Add 10 mL KI/EDTA until the solution turns rusty red.
5. Titrate with 0.1 N sodium thiosulfate to a pale yellow color.
6. Add 2 mL of starch indicator to turn the solution deep blue. If using strips. Hold the
indicator with a tong.
7. Continue to titrate with sodium thiosulfate until the solution becomes colorless for 30
seconds.

Calculation
Concentration of E-Pik (oz/gal) = (mL of 0.1 N Sodium thiosulfate) x 1.18
This should be around 16 oz/gal
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Running the deoxidizing phase

Procedure
This is done in room temperature. While the solution does not need to be heated up, it is a
moderately acidic solution.

1. Soak the cathode into the acidic solution for 5 minutes.


Cold water rinse
Equipment
1 L beaker
4 silver anodes

Procedure
1. Fill the 1 L beaker up to 0.8 L.
2. Submerge the cathode within the cold water for 5 minutes.

Plating
Vendor operating parameters:
Optimum Range
Silver Metal 2.4 oz/gal 2-2.5 oz/gal
pH 8.8 8.5-9.5
Temperature 68F 60-75F
Cathode current density 1 3 0.5 5 ASF
Anode current density -- 2-10 ASF
Agitation air agitation on the anodes,
plus cathode rod agitation
or air agitation on the
cathodes.

Table 5: Plating vendor specs.

Recommended parameter:
68F = 20 C
Room temp

Bath charge-up
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Equipment
4 L beaker

Material
45 % KOH
40% nitric acid (HNO
3
)
E-Brite
D.I. water
pH indicator

Procedure
To make a 3 L solution

1. Pour out 1.8 L of E-Brite solution into the beaker.
2. Add in 1.2 L of D.I. water
3. Use the pH indicator to find the pH of the solution
4. Adjust the pH of the solution to 9.0 with KOH solution or nitric acid.

Calculation

E-Brite contains 4 (oz/gal) of silver, the concentrate must be diluted with D.I. water
Use a percentage of 70% E-Brite, 30% D.I. water
0.264 gal = L
X L x 4 (oz/gal) x 0.264 (gal/L) => (Y oz/3 L) x (L/0.264 gal) => (Z oz/gal)
X = 1.8 L, so Y = (2.4 oz/gal)

Testing the bath
Equipment
25 mL pipet
125 mL Erlenmeyer flask

Material
0.1 N KSCN
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98% sulfuric acid (H
2
SO
4
)
Nitric acid (HNO
3
)
2% Ferric ammonium
D.I. water

Procedure
1. Transfer 10 mL of solution sample into a 125 mL Erlenmeyer flask
2. Add 50 mL of D.I. water
3. Add 2 mL of nitric acid, 2 mL of sulfuric acid
4. Heat up the solution to boil, and let it boil for 5 minutes.
5. Let cool the solution. Add 5 mL of ferric ammonium sulfate.
6. Titrate with 0.1 N KSCN until the solution turns light orange

Calculation

Concentration of silver = (mL KSCN) x 0.144

Running electroplating

The plating can be done without fume hood. Nevertheless, since the whole setup for pre-
cleaning and deoxidizing should be performed within a fume hood. It is best to plate within the
fume hood as well. Prolonged exposure to E-Brite silver solution can cause the absorption of
silver into the blood stream. Please wear gloves accordingly.

Equipment
DC power supply (up to 1 Amp)
Copper cathode
4 Silver anodes
4 L beaker

Material
E-Brite

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Procedure
Recommend using 3 ASF for both anode and cathode

Use the bath from the bath charging step. Refer the bath charging-up.

1. Take the target copper cathode from the cold water rinse.
2. Fit the 4 silver anodes onto the plating lid. Submerge all electrodes within the solution.
3. Turn the DC power supply on. Select current mode and switch up to 0.256 A.
4. Wait for the plating to take place. The amount of time required for 15 micron is.

Calculation
Current
ASF ampere per square foot (amp/ft^2)
Going from mm
2
to ft
2

Y ft
2
= (X mm
2
)

x (cm
2
/10 mm
2
) x (in
2
/2.54 cm
2
) x (ft
2
/12 in
2
)
When X = 16000 mm
2
, Y = 0.172 ft
2
Note: The surface area of the anode must be 4 times greater than the surface area of the copper.
3 (amp/ft
2
) x 0.172 ft
2
= 0.258 A

Cold water rinse
Equipment
1 L beaker

Procedure
1. Fill the 1 L beaker up to 0.8 L of cold water.
2. Submerge the cathode within the cold water for 5 minutes.
3. Wash the other electrodes.
D.I. water rinse
Equipment
1 L beaker

Material
24
D.I. water

Procedure
1. Fill the 1 L beaker up to 0.8 L. of D.I. water.
2. Submerge the cathode within the cold water for 5 minutes.
3. Wash the other electrodes.

Dry
Let it sit in the fume hood and let dry.

Conclusion

The plating machine currently produces silver plating albeit at less uniformity than had
expected. When examined under an optical microscope, the thickness of 15m has been achieved
using comparison to a 20 m gold thread. However, the distribution of silver upon the copper
surface has visible bumps. Further testing is required to isolate the cause of uniformity
Through this project, Ive gained the experience of researching, designing,
manufacturing, and operating the device from the start to finish. Ive gained skills in mechanical
machining, Solidworks CADDing, and mixing chemicals. The project has stretched my ability
beyond the bounds of engineering education, and has provided an overview of a challenging
engineering work.

Future work recommendation
The project could be expanded and in fact should incorporate these following elements in
the future to fix the problems of non-uniformity on the plating surface as recently observed on
the optical microscope. The first suggestion is a pH indicator, which could be implemented by
using the current calculation, derive from which, the transfer of ions from the silver anodes to the
cathodes. This will demonstrate the rate of the loss of ions within the solution. In order for this to
be implemented, a calculation needs to be done first to characterize the rate of ion loss, then,
repeated plating to test out the change of pH within the solution as compared to the calculation.

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The second recommendation of further work is to monitor the plating machine using the
serial communication capability of the Agilent voltage supply. This will involved the use of
LabView and a graphical interface program. It will monitor the loss of ions from the solution, as
well as the thickness of the deposition as predicted by the deposition equation. This is to be
implemented by a repeated trial of depositions and then characterize the deposition by thickness
measurement under the optical microscope, while varying the deposition time, the deposition
current, and the deoxidizing time as variables.

Appendix

List of Figures and Tables

Figure 1: Electroplating tank diagram
Figure 2: a) Target device. b) Target device dimensions
Figure 3: Layout of the setup
Figure 4: Illustrating solution level.

Table 1: Materials considered for tank
Table 2: Soak clean vendor specs.
Table 3: Electrolytic clean vendor specs
Table 4: Surface activation vendor specs.
Table 5: Plating vendor specs.
Table 6: Table of symbols, name, molar mass, and risk phrases

Percentage solution

1. % W/W gram of solute per 100 grams of solution
2. % W/V gram of solute per 100 mL of solution
3. % V/V mL of solute per 100 mL of solution

Molar
gmw of solute per 1 L of solution
26

Normal
gew of solute per 1 L of solution
or
normal = molar x valence

Chemical symbol and rating
It is strongly suggested to obtain the MSDN sheets for the handling of these materials.
Symbol Name Molar mass (g/mol) Risk phrases
HCl hydrochloric acid 36.46 R20 R21 R22 R36 R37 R38
H
2
SO
4
sulfuric acid 98.08 R23 R24 R25 R35 R36 R37
R38 R49
HNO
3
nitric acid 63.01 R8 R23 R24 R25 R34 R41
KI potassium iodide 166.00 R36 R38 R42 R43 R61
KOH potassium hydroxide 56.10564 R20 R21 R22 R35 R41
C
10
H
16
N
2
O
8
ethylenediaminetetraacetic
acid (EDTA)
292.25 R36
KSCN potassium thiocyanate 97.18 R22 R36 R37 R38.
Na
2
S
2
O
3
sodium thiosulfate 158.09774 R36 R37 R38
FeNH
4
(SO
4
)
2

12H
2
O
ferric ammonium sulfate R36 R37 R38
Table 6: Table of symbols, name, molar mass, and risk phrases

R20 Harmful by inhalation.
R21 Harmful in contact with skin
R22 Harmful if swallowed.
R23 Toxic by inhalation.
R24 Toxic in contact with skin.
R25 Toxic if swallowed.
R34 Causes burns.
R35 Causes severe burns.
R36 Irritating to eyes.
R37 Irritating to respiratory system.
R38 Irritating to skin.
R41 Risk of serious damage to the eyes.
R42 May cause sensitization by inhalation.
R43 May cause sensitization by skin contact.
R49 May cause cancer by inhalation.
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Original vendor summary


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Supplier tank design