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Development of Catalytic Activity Protocol for Electrochemical
Reduction of Carbon Dioxide

Surya Singh

Centre for the Environment
Indian Institute of Technology Guwahati
Guwahati, Assam – 781 039
Presentation Outline
Introduction

Idea behind the work

Development of Protocol

Validation

Results

References
Electrochemical Reduction of Carbon Dioxide

Breaches
400 ppm
on May
9th, 2013

Ref U.S. EIA, monthly energy review, Table 1.3, March 2012

Dec. 10-12, 2013

ICAER – 2013

3
Possible options for the mitigation of excess CO2

Decrease in fossil fuel consumption and other activities which result in CO2 emission

Effective use of technologies to reduce CO2 emission to the atmosphere

Capture CO2 and dump it in geologic or oceanic reservoirs

Utilize CO2 by converting it to either fuels or some other value added products, resulting in two
fold advantages:
a. Reduction in CO2 level
b. Reducing the dependency over conventional non-renewable fossil fuels, thus enhancing
energy security.

Dec. 10-12, 2013

ICAER – 2013

4
Utilization of CO2 for the production of value added products

(Ref. Viswanathan B., Proc. Ind. Acad. Sci., 70 A (3), 2004)

Dec. 10-12, 2013

ICAER – 2013

5
Why Electrochemical reduction of Carbon Dioxide ?

 Reactions can be carried
out at ambient temperature
and pressure conditions

 Co-reactant is Water

 Need of electrical energy can
be fulfilled using renewable
energy resources

(Source: Olah et al., JOC Perspective, 74 (2), 2009)

Dec. 10-12, 2013

ICAER – 2013

6
Electrochemical Reduction of Carbon Dioxide (ERC)

Anode

Cathode

Anode Reaction:
2H2O
4H+ + 2e- + O2
Cathode Reactions:
CO2 + 2H+ + 2eHCOOH
CO2 + 2H+ + 2eCO
+ H2O
CO2 + 6H+ + 6eCH3OH + H2O
CO2 + 8H+ + 8eCH4
+ 2H2O
Dec. 10-12, 2013

ICAER – 2013

Eo = - 1.23 V vs. SHE
Eo = - 0.225 V vs. SHE
Eo = - 0.103 V vs. SHE
Eo = + 0.031 V vs. SHE
Eo = + 0.169 V vs. SHE

7
Challenges to overcome

1

2

Activate this thermodynamically stable molecule

The actual electrolysis potential for CO2 reduction is
much more negative than the eq. potential

3

4

Product separation and analysis

5
Dec. 10-12, 2013

Simultaneous production of Hydrogen

Difficult to achieve the selectivity of products

ICAER – 2013

8
Use of ELECTROCATALYSTS

How to screen an electrocatalyst from
the group of many ?

Dec. 10-12, 2013

ICAER – 2013

9
Conventional Approach : Cyclic Voltammetry (CV)

Ex. Cu, Sn, CuO etc.
N2 Atmosphere: Aqueous KHCO3
solution, bubbled with N2 - pH 8.5
CO2 Atmosphere: Aqueous KHCO3
solution, saturated with CO2 - pH 7.5
Dec. 10-12, 2013

Ex. Mo2C etc.
Anomaly : Ag, Ni, Co3O4 etc.
ICAER – 2013

10
Development of Protocol

Dec. 10-12, 2013

ICAER – 2013

11
Select a probable electrocatalyst for ERC based upon literature and experience
Test its activity towards ERC (aqueous medium)
1st Test: In 0.5 M aqueous KHCO3, saturated with CO2 (pH 7.5)
Get LSV in presence and absence of catalyst
Electrocatalyst may not be
active for ERC
(particularly
in aqueous medium)

NO

YES

Current increased in presence of catalyst

Electrocatalyst may be active for ERC
INFERENCE

Increased current may be due to increased
H+ reduction / CO2 reduction or both
Test the electrocatalyst activity towards H+ reduction

2nd Test: In KOH aqueous solution (pH 7.5)
Get LSV in presence and absence of catalyst
H+

NO

Electrocatalyst is not active for
reduction INFERENCE
Electrocatalyst may be active only
towards ERC

Current increased in presence of catalyst

YES

Electrocatalyst is also active for H+
reduction
INFERENCE

Electrocatalytic activity has to be checked
esp. for CO2 reduction in absence of H+ ion

Test the electrocatalyst activity towards ERC (non aqueous medium)
3rd Test: In DMF, bubbled with CO2 (pH 7.5)
Get LSV in presence and absence of catalyst
Electrocatalyst is inactive for CO2
reduction

NO
Current increased in presence of catalyst

YES

Electrocatalyst may work for ERC
INFERENCE

Full Cell reaction can be attempted
Electrocatalysts Selection

Cu

Commercially
Purchased

Dec. 10-12, 2013

CuO

Synthesized
through Aqueous
Precipitation
method

Co3O4

Synthesized
through Polymer
Combustion
Route

ICAER – 2013

ZnO

Synthesized
through Aqueous
Precipitation
method

Mo2C

Commercially
Purchased

13
Characterization of the Electrocatalysts - XRD
ZnO

CuO

Mo2C

Dec. 10-12, 2013

ICAER – 2013

Co3O4

14
Characterization of the Electrocatalysts - FESEM

CuO

Mo2C
Dec. 10-12, 2013

ZnO

Co3O4
ICAER – 2013

15
Characterization of the Electrocatalysts – EDX & FTIR
CuO

Co3O4

Dec. 10-12, 2013

ICAER – 2013

ZnO

Co3O4

16
Characterization of the Electrocatalysts – BET surface area



9.9 m2/g



ZnO

15.9 m2/g



Mo2C

5.8 m2/g



Dec. 10-12, 2013

CuO

Co3O4

9.2 m2/g

ICAER – 2013

17
‘Cyclic Voltammetry’ tests using selected electrocatalysts

Cu

Mo2C

ZnO

CuO
Dec. 10-12, 2013

Co3O4
ICAER – 2013

18
‘Protocol Results’ using selected
electrocatalysts
Protocol
Results

Electrocatalysts

1st Test (% j)

2nd Test (% j)

3rd Test (% j)

Cu

Yes (146)

Yes (38)

Yes (52)

CuO

Yes (21)

Yes (13)

Yes (32)

ZnO

Yes (19)

Yes (18)

Yes (20)

Mo2C

No (~ 0)

Not Applicable

No (~ 0)

Co3O4

Yes (28)

Yes (21)

Yes (45)
1st Test: CO2 sat. Aq. KHCO3 solution
2nd Test: KOH solution
3rd Test: CO2 bubbled DMF

( j denotes the current density)
Dec. 10-12, 2013

ICAER – 2013

19
Comparison of the results of Proposed Protocol with CV test

Activity of Electrocatalysts
Electrocatalysts
CV

Cu

√

√

CuO

√

√

ZnO

~

√

Mo2C

X

X

Co3O4

Dec. 10-12, 2013

Proposed Protocol

X

√

ICAER – 2013

20
Full Cell Reaction using electrocatalysts
CO2 saturated
aq. KHCO3

Water
inlet

Gas chromatography (GC)

Cathode

Anode

High performance liquid
chromatography (HPLC)

Cathode
outlet
O2, H2O
outlet
Electrocatalysts

Electrolyte

Product

Yield (%)

CuO

Nafion

Methanol

8.7 %

ZnO

Nafion

Methanol

5.4%

Co3O4

Nafion

Formaldehyde

1.78%

Dec. 10-12, 2013

ICAER – 2013

21
Summary

Objective

The problem in quick
selection
of
an
electrocatalyst from a
group of many, was
identified as a major
issue in the field of
electrochemical
reduction of carbon
dioxide

Dec. 10-12, 2013

Protocol Development

A new protocol has been
developed for the quick
screening
of
electrocatalysts.

Validation

Results

Various electrocatalysts
were selected to validate
the protocol.

The protocol was
found valid for all the
electrocatalysts tested.

Electrocatalysts
were
characterized
physicochemically.

ICAER – 2013

22
Acknowledgements
 First and Foremost thanks to my supervisors Dr. Anil Verma & Dr. Chandan Mukherjee for
their sagacious guidance, suggestions and sustained encouragement.
 Thanks to the National Program on Carbon Sequestration Research, DST, New Delhi for the
financial support vide project grant number DST/IS-STAC/CO2-SR-139/12(G).
 Heartful gratitude to my research group members:
•
•
•
•
•
•

Ms. Lepakshi Barbora
Mr. Avijit Ghosh
Mr. Leela M. Aeshala
Mr. V. Shyam K. Yadav
Mr. Ehtesham Hussain
Mr. Rajamahendra Rapally
Thank You!!

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  • 1. Development of Catalytic Activity Protocol for Electrochemical Reduction of Carbon Dioxide Surya Singh Centre for the Environment Indian Institute of Technology Guwahati Guwahati, Assam – 781 039
  • 2. Presentation Outline Introduction Idea behind the work Development of Protocol Validation Results References
  • 3. Electrochemical Reduction of Carbon Dioxide Breaches 400 ppm on May 9th, 2013 Ref U.S. EIA, monthly energy review, Table 1.3, March 2012 Dec. 10-12, 2013 ICAER – 2013 3
  • 4. Possible options for the mitigation of excess CO2 Decrease in fossil fuel consumption and other activities which result in CO2 emission Effective use of technologies to reduce CO2 emission to the atmosphere Capture CO2 and dump it in geologic or oceanic reservoirs Utilize CO2 by converting it to either fuels or some other value added products, resulting in two fold advantages: a. Reduction in CO2 level b. Reducing the dependency over conventional non-renewable fossil fuels, thus enhancing energy security. Dec. 10-12, 2013 ICAER – 2013 4
  • 5. Utilization of CO2 for the production of value added products (Ref. Viswanathan B., Proc. Ind. Acad. Sci., 70 A (3), 2004) Dec. 10-12, 2013 ICAER – 2013 5
  • 6. Why Electrochemical reduction of Carbon Dioxide ?  Reactions can be carried out at ambient temperature and pressure conditions  Co-reactant is Water  Need of electrical energy can be fulfilled using renewable energy resources (Source: Olah et al., JOC Perspective, 74 (2), 2009) Dec. 10-12, 2013 ICAER – 2013 6
  • 7. Electrochemical Reduction of Carbon Dioxide (ERC) Anode Cathode Anode Reaction: 2H2O 4H+ + 2e- + O2 Cathode Reactions: CO2 + 2H+ + 2eHCOOH CO2 + 2H+ + 2eCO + H2O CO2 + 6H+ + 6eCH3OH + H2O CO2 + 8H+ + 8eCH4 + 2H2O Dec. 10-12, 2013 ICAER – 2013 Eo = - 1.23 V vs. SHE Eo = - 0.225 V vs. SHE Eo = - 0.103 V vs. SHE Eo = + 0.031 V vs. SHE Eo = + 0.169 V vs. SHE 7
  • 8. Challenges to overcome 1 2 Activate this thermodynamically stable molecule The actual electrolysis potential for CO2 reduction is much more negative than the eq. potential 3 4 Product separation and analysis 5 Dec. 10-12, 2013 Simultaneous production of Hydrogen Difficult to achieve the selectivity of products ICAER – 2013 8
  • 9. Use of ELECTROCATALYSTS How to screen an electrocatalyst from the group of many ? Dec. 10-12, 2013 ICAER – 2013 9
  • 10. Conventional Approach : Cyclic Voltammetry (CV) Ex. Cu, Sn, CuO etc. N2 Atmosphere: Aqueous KHCO3 solution, bubbled with N2 - pH 8.5 CO2 Atmosphere: Aqueous KHCO3 solution, saturated with CO2 - pH 7.5 Dec. 10-12, 2013 Ex. Mo2C etc. Anomaly : Ag, Ni, Co3O4 etc. ICAER – 2013 10
  • 11. Development of Protocol Dec. 10-12, 2013 ICAER – 2013 11
  • 12. Select a probable electrocatalyst for ERC based upon literature and experience Test its activity towards ERC (aqueous medium) 1st Test: In 0.5 M aqueous KHCO3, saturated with CO2 (pH 7.5) Get LSV in presence and absence of catalyst Electrocatalyst may not be active for ERC (particularly in aqueous medium) NO YES Current increased in presence of catalyst Electrocatalyst may be active for ERC INFERENCE Increased current may be due to increased H+ reduction / CO2 reduction or both Test the electrocatalyst activity towards H+ reduction 2nd Test: In KOH aqueous solution (pH 7.5) Get LSV in presence and absence of catalyst H+ NO Electrocatalyst is not active for reduction INFERENCE Electrocatalyst may be active only towards ERC Current increased in presence of catalyst YES Electrocatalyst is also active for H+ reduction INFERENCE Electrocatalytic activity has to be checked esp. for CO2 reduction in absence of H+ ion Test the electrocatalyst activity towards ERC (non aqueous medium) 3rd Test: In DMF, bubbled with CO2 (pH 7.5) Get LSV in presence and absence of catalyst Electrocatalyst is inactive for CO2 reduction NO Current increased in presence of catalyst YES Electrocatalyst may work for ERC INFERENCE Full Cell reaction can be attempted
  • 13. Electrocatalysts Selection Cu Commercially Purchased Dec. 10-12, 2013 CuO Synthesized through Aqueous Precipitation method Co3O4 Synthesized through Polymer Combustion Route ICAER – 2013 ZnO Synthesized through Aqueous Precipitation method Mo2C Commercially Purchased 13
  • 14. Characterization of the Electrocatalysts - XRD ZnO CuO Mo2C Dec. 10-12, 2013 ICAER – 2013 Co3O4 14
  • 15. Characterization of the Electrocatalysts - FESEM CuO Mo2C Dec. 10-12, 2013 ZnO Co3O4 ICAER – 2013 15
  • 16. Characterization of the Electrocatalysts – EDX & FTIR CuO Co3O4 Dec. 10-12, 2013 ICAER – 2013 ZnO Co3O4 16
  • 17. Characterization of the Electrocatalysts – BET surface area  9.9 m2/g  ZnO 15.9 m2/g  Mo2C 5.8 m2/g  Dec. 10-12, 2013 CuO Co3O4 9.2 m2/g ICAER – 2013 17
  • 18. ‘Cyclic Voltammetry’ tests using selected electrocatalysts Cu Mo2C ZnO CuO Dec. 10-12, 2013 Co3O4 ICAER – 2013 18
  • 19. ‘Protocol Results’ using selected electrocatalysts Protocol Results Electrocatalysts 1st Test (% j) 2nd Test (% j) 3rd Test (% j) Cu Yes (146) Yes (38) Yes (52) CuO Yes (21) Yes (13) Yes (32) ZnO Yes (19) Yes (18) Yes (20) Mo2C No (~ 0) Not Applicable No (~ 0) Co3O4 Yes (28) Yes (21) Yes (45) 1st Test: CO2 sat. Aq. KHCO3 solution 2nd Test: KOH solution 3rd Test: CO2 bubbled DMF ( j denotes the current density) Dec. 10-12, 2013 ICAER – 2013 19
  • 20. Comparison of the results of Proposed Protocol with CV test Activity of Electrocatalysts Electrocatalysts CV Cu √ √ CuO √ √ ZnO ~ √ Mo2C X X Co3O4 Dec. 10-12, 2013 Proposed Protocol X √ ICAER – 2013 20
  • 21. Full Cell Reaction using electrocatalysts CO2 saturated aq. KHCO3 Water inlet Gas chromatography (GC) Cathode Anode High performance liquid chromatography (HPLC) Cathode outlet O2, H2O outlet Electrocatalysts Electrolyte Product Yield (%) CuO Nafion Methanol 8.7 % ZnO Nafion Methanol 5.4% Co3O4 Nafion Formaldehyde 1.78% Dec. 10-12, 2013 ICAER – 2013 21
  • 22. Summary Objective The problem in quick selection of an electrocatalyst from a group of many, was identified as a major issue in the field of electrochemical reduction of carbon dioxide Dec. 10-12, 2013 Protocol Development A new protocol has been developed for the quick screening of electrocatalysts. Validation Results Various electrocatalysts were selected to validate the protocol. The protocol was found valid for all the electrocatalysts tested. Electrocatalysts were characterized physicochemically. ICAER – 2013 22
  • 23. Acknowledgements  First and Foremost thanks to my supervisors Dr. Anil Verma & Dr. Chandan Mukherjee for their sagacious guidance, suggestions and sustained encouragement.  Thanks to the National Program on Carbon Sequestration Research, DST, New Delhi for the financial support vide project grant number DST/IS-STAC/CO2-SR-139/12(G).  Heartful gratitude to my research group members: • • • • • • Ms. Lepakshi Barbora Mr. Avijit Ghosh Mr. Leela M. Aeshala Mr. V. Shyam K. Yadav Mr. Ehtesham Hussain Mr. Rajamahendra Rapally