In the last decade, a greater understanding of critical electrochemical transformations has been established, particularly those that involve water, hydrogen, and oxygen . The expansion of our understanding in this realm was only possible because of the use of critical electrochemical techniques. This has allowed researchers to not only explore a wider variety of catalysts, but explore them in greater detail.
To respond to the potential volume of exploration which may discover more cost-effective and renewable materials that are not at the stage of critical depletion, a systematic approach to analytical research is required.
Instrumentation for CV analysis of catalysts from Metrohm Autolab.
Experimental Goals and Procedure Selection
Exploring a new system
Determine the (E) stability window of the electrolyte 
Method: Perform CV measurement in broad voltage (E) window, using an inert electrode (e.g. glassy carbon) and investigate the general redox behavior of the electrocatalyst material.
Investigate the general redox behavior of the electrocatalyst material 
Method: Perform CV measurement in a broad voltage (E) window, using a well understood electrolyte and new electrocatalyst.
Determine the electrode surface area for quantitative comparisons [3–5]
Method: Various methods that are material dependent: using a well-defined surface reaction (e.g. stripping or oxide formation) or analysis of electrochemical double layer capacitance (Cdl).
Method: Perform repetitive CV measurements over several hundred cycles or during several days.
Probing a specific electrochemical reaction
Determine if a reaction is reversible (fast electron transfer kinetics), quasi reversible (slow kinetics), or irreversible (governed by other factors) [8, 9]
Method: Perform CV measurements at various scan rate values, then examine dependencies for the peak position (Epeak) and peak height (Ipeak) on the scan rate.
Combining CV with additional techniques to confirm results and deepen understanding
Determine the molecular structure of products or intermediates at a specific instance of the reaction [9–12]
Method: Perform CV measurement with in-situ spectroscopic determination (spectroelectrochemistry via UV/Vis/NIR or Raman spectroscopy).
Investigate material deposited or removed from the electrode surface during the electrochemical measurement 
Method: Measure the mass change at the electrode surface during a CV measurement using electrochemical quartz crystal microbalance (EQCM).
From action to reactions in the literature
Focal parameters for exploration:
1. Catalyst Microstructure
Research goal: Determine the electrode surface
Using microscope images combined with the Cdl (double layer capacitance) and ionomer coverage, the researchers were able to analyze and quantify their catalyst layer. They used CV to determine ionomer coverage over the carbon by comparing Cdl values (wet versus dry).
2. Transport Properties
Research goal: Investigate material deposited or removed from the electrode surface during the electrochemical measurement
Additional research investigating the electrode surface was performed with CV. Using a rotating disk electrode, the researchers were able to determine the gas transport resistance by measuring the ORR (oxygen reduction reaction). CV also allowed the determination of the Pt roughness factor.
3. I-V performance
Research goal: Use CV I-V to calculate the fuel cell performance
I-V performance is a typical measurement for the overall performance of the fuel cell. A potentiostat is needed to measure the actual I-V curve in order to determine the Pt loading so that the I-V performance can be interpreted and compared among various samples.
Your initial investigations with CV may not provide all of the answers at first glance, but you can then move on to more complex setups and experiments with complete insight.
Curious about electrochemistry?
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