Lab 3 – Electrodeposition

Background
Electrodeposition involves the deposition of a metal onto an object composed of a different metal.
Electroplating is a process that puts you in control. An electric current is used to reduce the cations in
the solution, forming a thin layer on a conductive material. This current is run from the anode to the
cathode, both of which are completely immersed in a salt solution, allowing electricity to flow through
the circuit. The direct current applied at the anode allows the metal ions to be oxidized, dissolving them
into the solution. These dissolved ions are then reduced at the cathode, which plates the metal ions onto
the conductive material. You can see this process in action in Figure 1 below, demonstrating your
precision and control over the electroplating process.

Figure 1. Electrodeposition setup of copper onto a brass electrode.

Electroplating is an incredibly precise and controlled technique, offering a fascinating level of control
over the surface composition. The thickness of the deposited layer can be finely tuned by adjusting the
operating conditions, such as the electric current and the rate of mixing of ions in the solution.

A common technique used in manufacturing microelectronics involves applying a patterned ‘mask’ on

an object to selectively block the deposition of metal so that deposition only occurs on the area left
exposed. This technique, known as photolithography, is a key step in the fabrication of microchips.
Figure 2 shows the deposition process: first, the mask is applied to the sample; then, the metal is
deposited selectively in the exposed area; and finally, the mask is removed using a solvent. This process
can be reversed by etching the metal from a precisely controlled area called electrochemical
micromachining. This technique is used to create intricate patterns and structures on microelectronic
devices, enhancing their functionality and performance.

Electroplating offers a level of control that extends to the micro/nanometre scale. As evidenced by the
SEM (scanning electron microscope) micrograph of an electrochemically machined component of an
electronic circuit board, this manufacturing technique allows for precise control of the surface structure
and composition, opening a world of possibilities in materials science and engineering.

Redox Reactions
Redox reactions, or oxidation-reduction reactions, describe the transfer of electrons between two
chemical species. These reactions are made up of two half-reactions, which always occur
simultaneously. The reduction half-reaction represents the gain of electrons to the oxidizing agent.
The oxidation half-reaction represents the loss of electrons to the reducing agent. A simple way to
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MSE 359/METE 355, Materials/Metallurgical Characterization Lab, Materials Engineering Department, KNUST, Kumasi
remember the difference between oxidation and reduction is to use the mnemonic ‘OIL RIG,’ which
stands for ‘oxidation is loss; reduction is gain,’ and represents the movement of the electrons. These
two ½ reactions will simplify the balanced net ionic equation when put together.

Figure 2. Left: An electrochemically etched piece or a circuit board Right: The process of depositing
metal on a surface.

Faraday’s Law
Using Faraday’s Law, the amount of anode material deposited on the cathode can be calculated:
𝑞 𝑤 𝐼𝑡
𝑛 = 𝑧𝐹, = 𝑧𝐹
𝑀
Where n = amount of material, mol, w = mass of material, g, M = molar mass of material, g/mol, I
= current, A, t = time, s, z = number of electrons, F=Faraday’s constant, 96485 C/mol

Methodology
Part 1 - Electroplate Nickel with Copper (2 electrode system)
▪ Clean your copper and nickel plates with steel wool.
▪ Weigh Nickel and copper plates and record masses.
▪ Connect the copper plate to the positive electrode with an alligator clip.
▪ Connect the Nickel plate to the negative electrode.
▪ Obtain 100 mL stock solution of 0.5 M Sulfuric acid.
▪ Place the metallic electrodes into a 100mL beaker with ~50mL of H2SO4. Make sure the
alligator clips stay out of the solution. (Do not let the electrodes a touch each other.)
▪ Turn on the power source and set the voltage to achieve a current of 0.6 amps.
▪ Remove the plates after 5 minutes, rinse with a DI bottle, rinse with acetone, and carefully dry
with a paper towel.
▪ Record the mass of the cathode and anode.
▪ Obtain a new plate and repeat part 1 twice with power source set to achieve currents of 0.2
amps and 0.4 amps. (Use the same solution)
▪ Dispose of waste in the proper container.

Part 2 - Electroplate nickel plate with copper using Potentiostat

▪ Obtain 50 mL of 0.1M copper sulfate solution, add ~ 7 mL of 0.5M H2SO4.
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MSE 359/METE 355, Materials/Metallurgical Characterization Lab, Materials Engineering Department, KNUST, Kumasi
 ▪ Repeat part 1 with this new solution using a nickel as the cathode, copper as the anode.
▪ Set voltage to achieve a current of ~0.4 amps.
Results and Discussion
1. Record the necessary data in the Tables provided below:

Table 1:
Dimensions Ni Plate Copper Plate
Length a (cm)
Width b (cm)
Thickness c (cm)
Area (cm2)

Table 2:
Deposition Voltage Sample Weight after Rate of Deposition
Current (A)
Time (mins) (V) Weight (g) deposition (g) (g/min)
10 0.2
20 0.4
20 0.6
40 0.8

2. Collect, plot, and analyze electrodeposition data from the electrochemical workstation

Lab Questions
1. What is the mass of the Cu deposited onto the Ni for each current (0.2, 0.4, 0.6). Calculate the
mass of Cu deposited on the Ni plate after 5 minutes for the following applied current:
(a) 0.2 amps
(b) 0.4 amps
(c) 0.6 amps
2. Why are the measured masses different from the calculated mass deposited? Include sources of
error in the measurement.
3. Using Part 2, based on the number of moles of anode material lost, how many moles should have
been electroplated onto the cathode? Does this match what you observed? If it doesn’t match,
explain why. Explain any unexpected observations in part II.
4. What affects the deposition rate? Prepare data tables for parts 1 and 2 in your lab notebook to
record: cathode, anode, initial masses of cathode and anode, applied current, deposition time, final
masses of cathode and anode, change in mass of cathode and anode, and key observations.
5. Write balanced redox reactions for electroplating Cu2+ onto Ni0
(a) What is the difference between spontaneous redox and nonspontaneous redox?
(b) Are the redox reactions in question 1 spontaneous? Explain.

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MSE 359/METE 355, Materials/Metallurgical Characterization Lab, Materials Engineering Department, KNUST, Kumasi