ANU Centre for Sustainable Energy Systems (CSES) Lab Tool-book

checked date: Feb 2009 by Soe Zin

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Silver Plating Full Procedure
WARNING: Silver plating uses a cyanide solution, which is potentially very dangerous. This
procedure must be carried out with the utmost care, and all users must have a full
understanding of the risks associated with it.
1. Background
Silver plating uses a silver anode and a silver cyanide plating solution to selectively plate
silver onto exposed regions of silicon on a solar cell or device. Silver plating can also be used
to thicken up silver which may already have been deposited onto surfaces. Plating can be
done either with the assistance of an electric circuit (electroplating), or with illumination (light-
assisted plating). Light-assisted plating is best-suited for plating n-type doped silicon.
2. Hazards & Safety Gear
Hazards:
Cyanide Solution: Silver Cyanide (AgCN) dissolved in aqueous Potassium Cyanide (KCN)
solution.
WARNING: Cyanide solution is extremely hazardous and must be treated with the highest
level of care at all times. Ensure that you have read the Risk Assessment for Silver Plating
and also the MSDS for the cyanide plating solution.
In most cases, cyanide poisoning causes a deceptively healthy pink to red skin color.
However, if a physical injury or lack of oxygen is involved, the skin color may be bluish.
Reddening of the eyes and pupil dilation are symptoms of cyanide poisoning. Cyanosis (blue
discoloration of the skin) tends to be associated with severe cyanide poisoning.
ALWAYS AVOID contact with acids Cyanide solution will react readily with acids to form
the lethal gas hydrogen cyanide. It is therefore extremely important to ensure that the cyanide
solution and any implements used with the cyanide solution NEVER come into contact with
any acids. Plated wafers must be thoroughly rinsed in DI water prior to leaving the silver
plating fumehood.

Low voltage electrical hazard: Take care using the power supply and exposed attachment
clips.

Safety Gear
Wear protective clothing, including boots, lab coat, sleeve protectors, plastic gloves and nitrile
gloves to prevent skin contact. Use full face shield and plastic apron wherever splashing is
possible. ALWAYS use nitrile gloves which are dedicated for the silver plating fumehood only:
these gloves must be clearly marked Cyanide Only. A set of sleeve protectors should also be
kept in the silver plating cabinet and marked Cyanide Only.

ANU Centre for Sustainable Energy Systems (CSES) Lab Tool-book
checked date: Feb 2009 by Soe Zin

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3. Equipment & Resources
The stock bottle of cyanide solution (a black 20L carboy) plus the three brighteners are all
stored in the locked cupboard below the silver plating fumehood. The key is located on
the key-board in Lab E127.
A made up plating solution is stored in a rectangular plastic tank or container, with a lid to
prevent excessive evaporation, in a plastic tray on the fumehood bench. There are also
four separate, numbered rinse buckets on the fumehood bench. These may be topped up
at any time with DI water.
Other equipment required includes the wafer jigs, set of tweezers, a set of pliers (can be
used for scraping off silver that has built up on jig contact arms which may be required
before each plating). These should be clearly marked Cyanide Only and should NOT BE
REMOVED from the cyanide plating fumehood.
For electroplating, a power supply (on shelves adjacent to fumehood) and wires with
connectors are required.
For light-assisted plating, a light source and power supply are required (located on
shelves adjacent to fumehood)
A labelled, sealable cyanide waste container should be located in the fumehood.


4. Procedures
4.1 Preparation of a new plating solution:
Ratios of additives for making up plating solution
Stock plating solution: 150 mL per litre of make-up volume
Brightener S: 5 mL per litre of make-up volume
Brightener T: 5 mL per litre of make-up volume
Brightener HT: 3 mL per litre of make-up volume
DI Water Remainder of make-up volume

1. Don appropriate safety gear, including plastic apron and nitrile gloves labeled to be
used for Cyanide Only. NEVER use gloves that have previously been used in other
fumehoods, and NEVER introduce Cyanide Only gloves into other fumehoods.
2. Fill the new or thoroughly cleaned plating tank / container with DI water to two-thirds
of the final plating volume required. (eg. If final volume is 4L, two-thirds is 2.67L)
3. Using a long pipette with rubber bulb, carefully transfer the required amount of
SILVREX Plating Solution (150ml per litre of final solution volume) to the tank /
container. Ensure that the solution never comes close to filling the pipette. (If final
volume is 4L, 600ml of Silvrex Solution to be added)
ANU Centre for Sustainable Energy Systems (CSES) Lab Tool-book
checked date: Feb 2009 by Soe Zin

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4. Rinse pipette thoroughly using the four rinse baths, followed by a running DI water
rinse and retain in fumehood.
5. After thoroughly mixing the brightener in the small bottle, using a pipette with rubber
bulb add the required amount of SILVREX S BRIGHTENER S to the solution (5mL
per litre of final solution volume if final volume is 4L, 20ml of Silvrex S Brightener S
to be added).
6. After thoroughly mixing the brightener in the small bottle, using a pipette with rubber
bulb add the required amount of SILVREX S BRIGHTENER T to the solution (5mL
per litre of final solution volume if final volume is 4L, 20ml of Silvrex S Brightener T
to be added).
7. After thoroughly mixing the brightener in the small bottle, using a pipette with rubber
bulb add the required amount of SILVREX S BRIGHTENER HT to the solution (3mL
per litre of final solution volume if final volume is 4L, 12ml of Silvrex S Brightener HT
to be added).
8. Adjust the solution to final volume with deionised water and mix thoroughly. The
cyanide solution is now ready to use.
9. On the Cyanide Register (on inside of fumehood cupboard door, next to stock solution
carboy) make sure that you now register the amount of cyanide solution taken from
the stock solution.

4.2 Topping up a depleted / partially evaporated plating solution:
From time to time the plating solution will need to be renewed, particularly as it gradually
evaporates over time. This is best done by adding additional plating solution, DI water, and a
little more of each of the brighteners. Simply do so according to the ratios and instructions
given in 4.1 Preparation of a new plating solution where the make-up volume is
calculated from the final desired volume and the current low volume.

4.3 Electroplating (manual control):
1. Don appropriate safety gear, including nitrile gloves labeled to be used for Cyanide
Only. NEVER use gloves that have previously been used in other fumehoods, and
NEVER introduce Cyanide Only gloves into other fumehoods.
2. Observe the safety precautions before using any silver plating solution.
3. If the four rinse buckets require topping up, carefully top up with DI water.
4. Very carefully remove lid from the plating solution and place lower side up and out of
the way, avoiding the spillage of drops from the lid onto the fumehood.
5. Ensure that the container is sitting securely on the stirrer assembly, and turn the
stirrer on.
6. Position the wafer to be plated on the jig provided, with metal contact touching to the
contact pad on the wafer. If the metal contact has become plated with silver it is a
ANU Centre for Sustainable Energy Systems (CSES) Lab Tool-book
checked date: Feb 2009 by Soe Zin

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good idea to clean this off using the pliers, before commencing with silver-plating. This
may be necessary for every use.
7. Place the jig on the handler and connect negative wire from the power supply to the
handler this will act as a cathode and make direct contact with contact pad on the
wafer.
8. Connect positive wire from the power supply to Silver Block immersed in the cyanide
solution this will act as an anode.
9. Gently lower the jig into the plating solution.
10. When you are ready to do plating, apply appropriate voltage and current and start
your timer. You will need to calculate required current and time for plating. Generally
speaking, 0.05mA at 0.3 volts will plate approximately 1 cubic micron per minute.
However, plating rate will vary from sample to sample. During plating, you should
observe bubbling effects in the solution as well as on the wafer.
11. When the plating time is up, switch off the power supply and disconnect the wires
connected to cathode and anode contacts.
12. Carefully remove the silver anode out of the cyanide solution and the jig out of the
handler, followed by rinsing thoroughly at least FOUR TIMES, in each successive,
numbered rinse bucket.
13. Once this rinsing is completed, carefully detach the wafer from the jig and using
tweezers give this wafer a further rinse in at least the last two rinse buckets and then
in gently running DI water. Immerse the silver anode in the 1
st
rinse bucket.
14. Blow dry the wafer using the N
2
gun or leave it to dry in the fumehood.
15. Now that the wafer is detached from the jig, also give the jig a further rinse in at least
the final two rinse buckets.
16. Remove the handler out of the cyanide tank / container and rinse thoroughly in each
of the FOUR rinse buckets. After rinsing, place the handler in 1
st
rinse bucket.
For Multiple wafer plating, repeat steps 6 through 15.
17. Using kimwipes, wipe clean any cyanide drips in the fume cupboard and dispose of
kimwipe in the labeled Cyanide Only disposal bottle.
18. When plating process is completed fully, turn off the stirrer and COVER THE
CYANIDE SOLUTION with lid tightly to prevent the solution from being evaporated.
19. Fill in your details in the log book / solution use record provided.

4.4 Light-assisted Plating:
1. Don appropriate safety gear, including nitrile gloves labeled to be used for Cyanide
Only. NEVER use gloves that have previously been used in other fumehoods, and
NEVER introduce Cyanide Only gloves into other fumehoods.
2. Observe the safety precautions before using any silver plating solution.
ANU Centre for Sustainable Energy Systems (CSES) Lab Tool-book
checked date: Feb 2009 by Soe Zin

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3. If the four rinse buckets require topping up, carefully top up with DI water.
4. Very carefully remove lid from the plating solution and place lower side up and out of
the way, avoiding the spillage of drops from the lid onto the fumehood.
5. Ensure that the container is sitting securely on the stirrer assembly, and turn the
stirrer on.
6. Now carefully position the light source next to the plating solution.
7. Position the wafer to be plated on the jig provided, with the surface (n+ contact) to be
light-plated facing upward and with the metal contact touching the back of wafer (p
contact).
8. Place the jig on the handler and gently lower the jig into the plating solution.
9. When you are ready to do plating, switch on the light source power supply to the
desired setting and start a timer. You will need to calculate required current and time
for plating. Generally speaking, a light source power supply setting of 120 volts will
plate approximately 1 cubic micron per minute. However, plating rate will differ from
sample to sample. During plating, you should observe bubbling effects in the solution
as well as on the wafer.
10. When the plating time is up, switch off the light source power supply.
11. Carefully remove the silver anode out of cyanide solution and jig out of the handler
and rinse thoroughly at least FOUR TIMES, in each successive, numbered rinse
bucket.
12. Once this rinsing is completed, carefully detach the wafer from the jig and using
tweezers give this wafer a further rinse in at least the last two rinse buckets and then
in gently running DI water. Immerse the silver anode in the 1
st
rinse bucket.
13. Blow dry the wafer using the N
2
gun or leave it to dry in the fumehood.
14. Now that the wafer is detached from the jig, also give the jig a further rinse in at least
the final two rinse buckets.
15. Remove the handler out of the cyanide tank / container and rinse thoroughly in each
of the FOUR rinse buckets. After rinsing, place the handler in 1
st
rinse bucket
For Multiple wafer plating, repeat steps 7 through 14.
16. Remove light source to the shelves adjacent to the fumehood. If any drips have been
observed to land on the light source then it will require thorough cleaning prior to
being removed from the fumehood and stored on the adjacent shelves.
17. Using kimwipes, wipe clean any cyanide drips in the fume cupboard and dispose of
kimwipe in the labeled Cyanide Only disposal bottle.
18. When plating process is completed fully, turn off the stirrer and COVER THE
CYANIDE SOLUTION with lid tightly to prevent the solution from being evaporated.
19. Fill in your details in the log book / solution use record provided.

ANU Centre for Sustainable Energy Systems (CSES) Lab Tool-book
checked date: Feb 2009 by Soe Zin

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5. Clean Up and Waste Disposal
Storage
Keep plating solution currently in use in a tightly closed container, stored in a cool, dry and
ventilated area. Protect against physical damage. Separate from incompatibles. Proper use
and maintenance of protective equipment is essential. Stock solution and brighteners should
be stored separately in locked cupboard below fumehood.
Disposal of old Plating Solution
Disposal of plating solution should only be required occasionally. In the event that the
plating solution needs to be completely disposed of, it can be poured into a clearly labelled
Cyanide Plating Solution waste bottle and locked in the fumehood cupboard, with
collection by waste-disposal contractors then arranged.
EXTREME CARE must be exercised when performing this task. It must be done in the
presence / with the help of a second lab user. Make sure you plan everything before
commencing (fumehood layout etc), and if you are in any doubt about performing this
operation safely, DO NOT do it.
1. Ensure that the gas boost in the fumehood is on.
2. Don appropriate safety gear, including full face shield, plastic apron and nitrile gloves
labeled to be used for Cyanide Only. NEVER use gloves that have previously been
used in other fumehoods, and NEVER introduce Cyanide Only gloves into other
fumehoods.
3. Very carefully remove lid from the plating solution and place lower side up and out of
the way, avoiding the spillage of drops from the lid onto the fumehood. If there are lots
of drips on the lid, it should be rinsed in the four, successively numbered DI rinse
buckets.
4. Pick up solution tank / container, ensuring you have a reliable grip, and gently pour
solution from into an appropriate waste bottle or carboy. Avoid pouring too fast, and
use a funnel (it will need to be dedicated to cyanide plating solution use only) if
required.
5. Cap the waste bottle / carboy and clearly label it.
6. The plating tank / container may be rinsed using moderate amounts of DI water,
however this must be poured into the rinse buckets and NOT down the sink. If a
funnel was used, it should also be rinsed using the rinse buckets. A final rinse under
running DI is acceptable.
7. If there are any drops spilled in the fumehood, carefully wipe these up using kimwipes
and dispose of in the appropriate solid waste bottle.
8. Lock the waste container in the cyanide fumehood cupboard and notify others
(particularly Nina de Caritat) that waste collection is required.

Disposal of Rinse Water
ANU Centre for Sustainable Energy Systems (CSES) Lab Tool-book
checked date: Feb 2009 by Soe Zin

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Do not drain the rinse water into the sink. After some time the 1
st
rinse bucket can be
deemed to have been used too much (generaly when it has turned noticeably yellow); it can
then be set aside and left to evaporate (may take up to a week), leaving solid cyanide
compounds behind. It is then easiest to put a sealed lid on the rinse bucket and appropriately
disposing of it as solid cyanide waste (collected by waste disposal contractors). A new rinse
bucket can then be instituted as the 4
th
rinse bucket and the remainder moved up the order.

6. Troubleshooting
Plating rates will depend on several factors. It may be wise to consult other users about the
best settings to use for a given metalisation area