**2.2 Electrochemical CO2 reduction reaction**

For CO2RR an H-shaped electrochemical cell was used which has 2-chambers (cathodic and anodic sections) that were connected with membrane Nafion 117 as seen in **Figure 5**. CO2 gas was inserted into the cathodic section for the reduction process. In this method, electrocatalyst, reference electrodes (Ag/AgCl), and CO2 saturated cathodic electrolyte were in the cathodic part, where CO2RR happened, in the other part, the counter electrode (graphite) and anodic electrolyte (0.1 M H2SO4) were placed where the oxidation occurred. It was, therefore, predicted that SYNGAS (H2 + CO) and coke would form in the cathodic portion, and O2 would be produced in the anodic portion. Working, reference, and counter electrodes (WE, RE, and CE), were linked to the Autolab potentiostat device (Model: PGSTAT128N) to inspect potential and current records. A gas bag was attached to the exhaust to collect products for gas chromatography to characterize gases. Images of the catalyst morphologies were examined utilizing SEM. The catalysts were analyzed by EDX for coke formation and electrocatalyst surface compositions.

#### **Figure 4.**

*Electrodeposition setup for Zn-Ni coatings, (1) counter electrode, (2) reference electrode (3) working electrode, (4) thermometer.*

*Investigation of Zn/Ni-Based Electrocatalysts for Electrochemical Conversion of CO2 to SYNGAS DOI: http://dx.doi.org/10.5772/intechopen.95626*

**Figure 5.**

*Cell setup for electrochemical CO2RR by Zn-Ni electrocatalyst, graphite CE, 0.1 M KCl (cathodic solution), H2SO4 (anodic solution) and Ag/AgCl RE.*
