In-situ Electrochemical Infrared Spectroscopy Analytical Service

Overview

In-situ Electrochemical Infrared Spectroscopy is a powerful analytical technique that combines infrared (IR) spectroscopy with electrochemical methods to study surface and interfacial processes in real-time. It enables the detection and identification of molecular species adsorbed on electrode surfaces or present in the electrolyte during electrochemical reactions. By monitoring IR absorption peaks, researchers can gain insights into reaction mechanisms, intermediate species, and structural changes of materials under various applied potentials or currents. This technique is widely used in fields such as electrocatalysis, energy storage (e.g., batteries and fuel cells), and corrosion science.

Results Display

Reference: http://doi.org/10.1073/pnas.2318853121

To gain a molecular-level understanding of the reaction mechanism during the EG-to-GA conversion process, the authors conducted in-situ electrochemical infrared spectroscopy using a Thermo Nicolet 8700 equipped with an MCT detector cooled by liquid nitrogen. In-situ Fourier-transform infrared (FTIR) spectra were recorded in 1.0 M KOH and 1.0 M EG at 100 mV intervals over a potential range of 0 to 1.2 V (vs. RHE).

The peak at 1,660 cm⁻¹ corresponds to the 2-hydroxyacetyl (*OC-CH₂OH) intermediate, identified as a key intermediate in the EG-to-GA conversion process. The peak at 1,236 cm⁻¹ is attributed to the C-O stretching vibration of GA, while the peak at 1,411 cm⁻¹ corresponds to the symmetric stretching vibration of COO⁻ in GA. The peaks at 1,326 and 1,580 cm⁻¹ are related to the symmetric and asymmetric stretching of COO⁻ in GA, and the peak at 1,076 cm⁻¹ is attributed to the aldehyde (-CHO) stretching vibrations from glyoxal and GA species. Additionally, the spectral bands at 1,307 and 1,340 cm⁻¹ are associated with oxalate and carbonate (CO₃²⁻).

As shown in Figures E and F, the bands at 1,076 and 1,580 cm⁻¹ on Pd₆₇Ag₃₃ appeared at 0.5 V vs. RHE, which is lower than that on Pd (0.6 V vs. RHE), indicating that Pd₆₇Ag₃₃ exhibits a reduced energy barrier during the EG-to-GA conversion process. A comparison of the in-situ FTIR spectra of Pd and Pd₆₇Ag₃₃ revealed that the signals for GA (1,076, 1,236, 1,326, 1,411, and 1,580 cm⁻¹) were significantly enhanced on Pd₆₇Ag₃₃, while the intensity of bands associated with undesirable by-products (1,307 and 1,340 cm⁻¹) showed no significant change.

This result further highlights the improved GA selectivity on Pd₆₇Ag₃₃, consistent with the NMR results.

Sample Requirement

For electrocatalytic systems:

• Powder samples: Prepare at least 20 mg.
• Electrode sheets: Dimensions should be 10 × 10 mm, with a thickness not exceeding 1 mm. The surface must be dense and smooth.

For battery systems:

• Powder samples: Prepare at least 100 mg.

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Analytical Service Minimum order requirement: $250 per order. A $200 handling fee will be applied if order is below $250.

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