department of interface chemistry and surface engineering electrocatalysis group düsseldorf,...

Department of Interface Chemistry and Surface EngineeringElectrocatalysis GroupDüsseldorf, Germany

International Conference on Combinatorial Materials Research, Ghent 02.06.2015

Jan–Philipp Grote, Aleksandar R. Zeradjanin, Serhiy Cherevko,Karl J.J. Mayrhofer

E-mail: [email protected]

Electrochemical CO2 Reduction

A Combinatorial High-Throughput Approach for Catalytic Activity, Stability and Selectivity Investigations

Max-Planck-Institut für Eisenforschung GmbH, Germany International Conference on Combinatorial Materials Research, Ghent 02.06.2015

Intro

Motivation

Electrolyte Ions

Aqueos- / non-aqueous ElectrolytesSolved gases

pH Impurities

Operation conditionsPotential / current

EC techniqueTemperature

CatalystCompositionMorphology

Surface oxide Deposition

of impurities

Additional analysisDissolution

Product evolution

Motivation SFC SFC-ICP-MS SFC-OLEMS Conclusion


Intro

Scanning flow cell

Electrolytesupply

Counter electrode

Electrolyteoutlet

Reference electrode

Silicon sealing

2mmWorking electrode

Ar

Ar

Channel diameter: 0.2/0.4/1/3 mm

Flow rate: 50-200 μl/min

• CE: Pt-wire or C-rod

• WE area: 0.13/0.25/1.1/10mm2

• RE: Ag/AgCl/3M KCl

C. a. Laska et al., Electrochim. Acta, 159, 198–209 (2015)



Intro

Fast screening of high surface area cats

0.5 mm1 mm



Intro

SFC - Fast Screening of Alloys

Prof. Ludwig, Ruhr-Universität Bochum, Institute of Materials, Faculty of Mechanical Engineering

CuCo

4-inch Si-wafer

Argon atmosphere

Magnetron sputter depositionCu/Co Alloy



Intro

SFC-ICP-MS

Pt-Cu alloy

Oxidati

onReducti

on

A. Schuppert, A.Topalov, A. Savan, A. Ludwig, and K. J. J. Mayrhofer, ChemElectroChem, 1, 358–361 (2014). A. A. Topalov et al., Angew. Chem. Int. Ed. Engl., 51, 12613–5 (2012).



Intro

SFC-Online Electrochemical Mass Spectrometer

Stability Selectivity

J.-P. Grote, A. R. Zeradjanin, S. Cherevko, and K. J. J. Mayrhofer, Rev. Sci. Instrum., 85, 104101 (2014)



Intro

SFC-OLEMSMotivation SFC SFC-ICP-MS SFC-OLEMS Conclusion


Intro

SFC-OLEMS

J.-P. Grote, A. R. Zeradjanin, S. Cherevko, and K. J. J. Mayrhofer, Rev. Sci. Instrum., 85, 104101 (2014)



Intro

CO2 reduction

Pd, Hg, In, Sn, Cd, Tl, Bi

Cu

Au, Ag, Zn

Ni,Fe, Pt, Ti, Ga, Co

HCOO-

CO

H2

Hydrocarbons

CO2

"Carbon cycle" by Diagram adapted from U.S. DOE, Biological and Environmental Research Information System. - http://earthobservatory.nasa.gov/Features/CarbonCycle/



Intro

Cu-Co alloys

Cu-Coalloy

Cu a

t %

Ethylene Alcohols

MethaneHydrogen



Intro

Cu and Cu alloy oxides

Brass

Brass ox



Intro

Carbon corrosionMotivation SFC SFC-ICP-MS SFC-OLEMS Conclusion


Intro

SFC-OLEMS for high surface area cats

2 mm3 mm



Intro

Carbon corrosionMotivation SFC SFC-ICP-MS SFC-OLEMS Conclusion


Intro

Summary

Scanning flow cell• Automated:

• Potentiostat control• Position change• Electrolyte change• Purging gas control

• Defined surface area for reproducible electrochemistry• Temperature control

SFC-ICP-MS for dissolution studies

• High sensitive multi element analysis• Relation between potential and

dissolution• Quantitative results

SFC-OLEMS for selectivity studies

• Direct detection of volatile products• Response time below two seconds• Semi-quantitative results



Intro

Thanks for your attention!

Electrocatalysis Group from Max-Planck-Institut für Eisenforschung

department of interface chemistry and surface engineering electrocatalysis group düsseldorf,...

Documents

intro sfcicp

ms sfcolems conclusion

institute of materials

janphilipp grote

serhiy cherevko

mayrhofer email

flow rate

electrode ar channel