Thin Layer Pool In-Situ Differential Electrochemical Cell

Differential Electrochemical Mass Spectrometry (DEMS) is an in-situ electrochemical method that provides qualitative and quantitative information about the interface by detecting volatile products, making it an indispensable tool for studying electrochemical reaction mechanisms. The DEMS system combines an electrochemical reaction setup with a mass spectrometer, where volatile products generated from the electrochemical reaction pass through a hydrophobic and permeable membrane interface into the vacuum system of the mass spectrometer. The mass spectrometer then measures the current of different mass-to-charge ratio ions as a function of time. Cyclic Voltammetry (CV) is a commonly used electrochemical technique in the study of reaction mechanisms, and it provides rich electrochemical information from the obtained CV curves. Therefore, CV is frequently employed in DEMS studies. In DEMS-based electrochemical research, the ion current signal of the volatile products generated during the CV scan is detected by the mass spectrometer as a function of time. The transformation of the time axis to the potential axis provides the Mass Spectrometric Cyclic Voltammetry (MSCV) graph, which offers more comprehensive and in-depth information for studying the mechanisms of electrocatalytic reactions.

Figure 1: Working principle of the thin layer pool

Performance advantages:

1. High collection efficiency and sensitivity.

2. Proton exchange membrane can be added to avoid interference from electrode products.

3. Suitable for catalytic materials with different supports, such as carbon paper and foam copper.

4. Option for a concentric or eccentric design.

Specific applications include:

1. Instantaneous detection of gas-phase products (CO, CH₄, C₂H₄, CH₃OH, etc.) in CO₂ electrocatalytic reduction, as well as relative Faradaic efficiency determination.

2. In-situ detection of intermediate or final products (NO, N₂O, NH₂OH, NH₃, N₂, etc.) in nitrate electrocatalytic reduction.

3. Confirmation of the reaction mechanism in the oxygen evolution reaction (OER) of water electrolysis using isotopic labeling of 18O, LOM, or AEM.

4. Instantaneous detection and current efficiency calculation of intermediate or final products (HCHO, HCOOH, CO, etc.) in methanol electrooxidation reaction.

5. Mechanistic analysis of hydrogen evolution reaction (HER) using hydrogen isotope labeling and hydrogen gas evolution.

6. Evaluation of carbon material stability (CO and CO₂ detection under high potential).

7. Other applications such as photocatalysis, photoelectrocatalysis, oxygen reduction, hydroxide production, chlorine gas evolution, organic electrosynthesis, etc.

Application case:

1. Detection of intermediates in nitrate electroreduction.

Angew. Chem. Int. Ed. 10.1002/anie.201915992

 2. Electrolysis of water with OER isotope labeling ¹⁸O to confirm LOM or AEM reaction mechanism.

J. Am. Chem. Soc. 2021, 143, 17, 6482-6490

3. Methanol electrocatalytic oxidation reaction.

Journal of Power Sources 509 (2021) 230397

4. Hydrogen isotope labeling for mechanistic analysis of Hydrogen Evolution Reaction (HER).

Nature catalysis, 2022,5,66-73

5. Electrochemical reduction of CO₂.

ACS catal. 2019,9,1383-1388

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Journal of Catalysis. 2020, 384, 199-207

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Cell Reports Physical Science. 2021, 2, 100583

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Energy Storage Materials. 2021, 42, 618-627

ACS Nano. 2021, 15, 9841–9850

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Adv. Funct. Mater. 2022, 2112501

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ACS Appl. Mater. Interfaces. 2022, 14, 18561-18569

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ACS Appl. Energy Mater. 2020, 3, 12423-12432

Nat Commun. 2022, 13, 1123

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ACS Appl. Mater. Interfaces. 2022, 14, 5308−5317

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Nat. Commun. 2021, 12, 5267

Nat. Commun. 2020, 11, 5519

Angew. Chem. Int. Ed. 2020, 59, 23061−23066

ACS Nano. 2021, 15, 8407−8417

Adv. Sci. 2022, 2104841

J. Am. Chem. Soc. 2022, 144, 3106-3116

Adv. Funct. Mater. 2022, 2113235

Journal of Energy Chemistry. 2022, 64, 511-519

Energy Environ. Sci. 2020, 13, 2540-2548

J. Mater. Chem. A. 2020, 8, 22754-22762

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ACS Appl. Mater.Interfaces. 2021, 13, 12159-12168

ACS Central Science 2021, 7, 175-182

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Journal of Power Sources. 2021, 495, 229782

Energy Storage Materials. 2021, 38, 130-140

Chem. Mater. 2020, 32, 9404-9414

Energy Storage Materials. 2021, 39, 60-69

Adv. Funct. Mater. 2021, 31, 2101423

Applied Surface Science. 2021, 565, 150612

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Chemical Engineering Journal. 2021, 426, 131101

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Journal of Materials Chemistry A. 2021, 9, 19922-19931

Small. 2021, 17, 2100642