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Abstract:

For biomedical devices, the purpose of an electrode is used as a means of gathering/recording

data from different systems. The following research focuses on characterizing the properties of
various electrodes [Gold (Au), Iridium Oxide (IrOx), and Silver/Silver Chloride] that can be used
in biomedical applications such as a customized micro-device. Several tests were performed to
characterize the three different types of electrodes including: measuring impedance, cyclic
voltammetry, and measuring potential levels signifying different pH levels for this micro-device.
The impedance measurement test was performed through an open circuit to detect resistance
measurements through a set range of frequencies resulting in the Au electrode containing an
average impedance of 5.79 103 while the electroplated IrOx electrode had 8.71 102 ,
picking up less background noise due to its higher electrical resistance. The Cyclic Voltammetry
test (used for measuring charge capacity) resulted in the tested devices falling in between the
charge capacity range of 2.31 107 to 4.80 108 Amps/2 . Lastly, a test to evaluate the
performance of the electrodes stability and durability in different pH buffer solutions was given
to show any differences in potential when compared to a commercial electrode. These electrodes
managed to remain stable throughout the duration of the tests, despite minor differences. With
the classification of these various electrodes, devices can be properly suited for biomedical
purposes and are able to receive sufficient data without causing any harm or other technical
faults.

Introduction:

In a biomedical device, the working electrode is used to detect any bioelectric/electric

signals generated from any system or solution, and can even stimulate a system upon

implantation. With these electrodes in action, proper diagnoses are given, certain illnesses can be

prevented, and any deficient activity can be stimulated. These electrodes are often used in many

micro-devices, including: cochlear implants, neural implants, and even pH sensors. This research

is focused on the characterization of different types electrodes in order to determine which is best

suited for recording as well as stability for a customized micro-device over a long period of time.

The electrodes used in this experiment are: Gold (Au), Iridium Oxide (IrOx) after being

electroplated (a process which bonds ions from a solution onto any surface), and Silver

electroplated with a Silver Chloride layer (Ag/AgCl). The characterization test for these
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electrodes will include: electrical impedance tests, cyclic voltammetry, and pH readings from the

custom micro-device.

Figure 1. The Fabricated pH Micro-device with Au Electrode

Figure 1 displays the custom micro-device with a working electrode (Au). This device

was design through AutoCAD software and created via microfabrication on a silicon disc. Once

fully assembled, this device will serve as a micro pH sensor for other research projects at Wayne

State University.

Electrical Impedance:

The first of these electrode tests was the electrical impedance test. Electrical impedance

serves as the ratio measurement of the voltage applied to a metal over the amount of current

generated in an AC (alternating current) circuit. For an electrode, having a lower impedance

level is significant when monitoring any electric reading because more background noise is

reduced, thus creating a higher signal to noise ratio. Another factor in impedance tests includes

the area of an electrode, in which the largest area possible can help give the lowest impedance

measurement since it the flow of electrons will be much easier. The area of each working
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electrode for this micro-device is 0.081692 . The configuration for this circuit is shown in the

figure below.

Figure 2. The Electrical Impedance Measurement Setup

Figure 2 displays the setup given to record the impedance data. The LCR Meter is used to

generate different frequencies (in kHz) and receive impedance measurements over a period of

time. The working electrode (indicated as the black object connected to the red wire), 1X

Phosphate Buffer Saline (PBS) aqueous solution, and a Platinum counter electrode (the grey

object connected to the black wire) are all used to help create an open AC circuit for this test.

The PBS aqueous solution was used for this experiment as a means to replicate fluids found in

the human body. The following test was done to compare the difference in impedance levels

between the Au and IrOx working electrodes for the micro-device. The data was collected

through a LabView application modified to measure impedance levels and to control the LCR

Meter. The numbers generated were put into a Microsoft Excel document and would later be

turned into a graph comparing the two results.

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Figure 3. Impedance Measurements of Au and IrOx Electrodes

Figure 3 displays the results of the impedance test between the two electrodes through a

frequency range of .2 20 kHz. On average, the Au electrode had an impedance measurement of

5.79 103 while the IrOx electrode generated an impedance of 8.71 102 . The reason as

to why the IrOx electrode tends to have a lower impedance level is because the IrOx electrode

has a very rough surface and has a much more effective electrochemical reaction with the PBS

(aq); whereas, the Au electrode is fairly smooth, causing less of a reaction to occur and more

background noise to be generated in the data collection.

Cyclic Voltammetry:

The next for the electrodes is the Cyclic Voltammetry test. This process shows where

current is developed in an electric cell when voltage is within an active range. This process

measures the current density over the amount of voltage, giving the result in . The Cyclic
2

Voltammetry test uses three types of electrodes: the working (IrOx electrode), the reference (a

commercial electrode), and a counter electrode (the Platinum piece). Current will be generated

through a high powered cell, while PBS (aq) will be used to help give an even current flow

throughout the circuit. A diagram of the circuit can be seen in Figure 4.

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Figure 4. Setup of Cyclic Voltammetry Test

The data was collected through the PowerSuite program, generating 50 test cycles over the span

of two hours. A graph would be generated to see if the electrode generated current efficiently.

Figure 5. Cyclic Voltammetry Test Result for IrOx Electrode (Cycle #5)

Figure 5 displays the results of the Cyclic Voltammetry test through one of its many

cycles. The current density range was given from 2.31 107 to 4.80 108 as the
2

voltage ranged from 0 to .575 V. As the voltage increases, the electrode undergoes an oxidation

reaction, losing the electrons of in the cell; however, as voltage decreases, the electrode reobtains

the electrons from the solution in a process known as the reduction reaction. The remaining

cycles similarly followed this trend as shown in Figure 5, signifying that the IrOx electrode

obtains the same current density range over time.

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pH Measurement:

One of the many biomedical applications that electrodes are involved in is pH level

testing. Different pH levels are known to generate different voltage levels, allowing the working

electrodes in the sensor of the pH device to display the correct readings upon detection. The

custom micro-device in this research consists of two types of electrodes: the working (IrOx) and

a custom reference (Ag/AgCl) which will both be compared to a commercial reference electrode

in this experiment. The test also compares the device to the commercial electrode through the pH

levels: 4, 7, and 10 through the setup shown below.

Figure 6. pH Test Setup

Figure 6 displays the setup for this test comparing the micro-device electrodes to the

commercial reference electrode. An electrometer is used to record the voltage. pH levels were

changed after each test and the data is shown through two different graphs comparing the two

different electrodes in the device.

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Figure 7. Potential Differences in Reference (Ag/AgCl) and Working (IrOx) Electrodes

compared to a Commercial Reference Electrode

Figure 7 gives the potential differences between both electrodes in the micro-device and

the commercial reference electrode. The graph on the left displays the difference between the

custom and commercial reference electrodes. The overall job of the reference is to make sure the

working electrode is able to properly read measurements. According to this data, the electrode is

able to get a more stable reading for all pH levels once a longer period of time has passed;

however, in the graph indicated on the right, the working electrode gives a very distinct and

consistent reading of the different pH levels and properly aligns the potential differences with the

different pH levels.

Conclusion:

The different electrodes were successfully characterized for both recording and

stimulation processes through the processes of impedance measurement, cyclic voltammetry, and

pH measurement serving as a biomedical application. These tests indicated that the custom

working electrode (IrOx) is the successful candidate for further biomedical application

experimentation. The device itself will be further modified and tested in other research projects

by different graduate students. The IrOx working electrode can be further used in experiments
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such as reading brainwave activity (neural signals), monitoring cochlear activity within humans

or animals, and even detecting the pH reading of bodily fluids of a being or other organism.

These experiments can give possible indication of its efficiency and durability over elongated

periods of time.
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Engineering Annu. Rev. Biomed. Eng. 10.1 (2008): 275-309. Web.

Franks, W., I. Schenker, P. Schmutz, and A. Hierlemann. "Impedance Characterization and

Modeling of Electrodes for Biomedical Applications. IEEE Transactions on

Biomedical Engineering IEEE Trans. Biomed. Eng.52.7 (2005): 1295-302. Web.

Grupioni, A.A.F, E. Arashiro, and T.A.F Lassali. "Voltammetric Characterization of an Iridium

Oxide-based System: The Pseudocapacitive Nature of the Ir0.3Mn0.7O2

Electrode." Electrochimica Acta 48.4 (2002): 407-18. Web.

Kim, Eric. Development of Advanced Multifunctional Neural Interface Devices. Wayne State

University. 2016. Print.

Nave, R. "Impedance." HyperPhysics. July-Aug. 2000. Web. 21 July 2016.

<http://hyperphysics.phy-astr.gsu.edu/hbase/electric/imped.html#c4>.

Neuman, M. R. Biopotential Electrodes. The Biomedical Engineering Handbook: Second

Edition. Boca Raton: CRC Press LLC, 2000. Web.