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Catalyst materials for solar refineries, synthetic fuels and
procedures for a circular economy of the CO2
J.R.Morante
IREC, Catalonia Institute for Energy Research, Plaça de les Dones de Negre,1.
Sant Adrià del Besòs, 08930. Spain.
Department of Electronics, University of Barcelona, C/Martí i Franquès,1.
Barcelona,08028. Spain.
H2
O2
Nowadays, the circular economy of carbon dioxide constitutes
one of the major world challenges.
Climatic change
CO2 emissions
The conversion of CO2 into value-added chemicals and/or fuels, using
renewable energy and earth-abundant elements as well as environmental
friendly materials is a key priority.
 Carbon dioxide closed loop in which this molecule is captured,
reduced and oxidized continuously defining an ideal circular
economy of the CO2
Fossil gas
CO2 emissions
Methanation based on
Paul Sabatier reactor.
Closed loop CO2-CH4
 Carbon dioxide reduction by thermochemical or plasma
procedures which are open new alternatives to the
methanation process
Patent: P201530109
300mg of catalyst,
corresponding to an GHSV of
20000, the reactor is supplied
with a mixture of carbon dioxide
and hydrogen (20% vol CO2)
with a total flow rate of 12000
ml/h), at atmospheric pressure
and at temperature of 20°C
Journal of CO₂ Utilization 26 (2018) 202–211
EELS chemical composition maps obtained from the red
rectangled area of the STEM-HAADF micrograph. Individual Ce
(red), Zr (green) and Ni (blue) maps and their composite. It
should be noted here that we have normalized the intensity
values of the maps to that of Ce to have a better comparison
Mesoporous
Bioconversion: Synthetic natural gas production from biogas in
a waste water treatment plant
In collaboration with Naturgy
programa RIS3CAT
ENERGY CONVERSION AND MANAGEMENT
162 pp 218-224 (2018)
Demonstration unit [Sabadell (Barcelona) Spain)
Digestor
GasometerBiogas
Methanation unit
CO2 + 4H2 –> CH4 + 2H2O
Alkaline electrolyzer
37 kWh
Biogas source (55-65% CH4)
H2S cleaning
CH4
CO2
CO2 source
10 Nm3/h
Methanation reactors
Compact
reactor technology
Quick start-up
and shut-down times
Load-flexibility
T depends on time, length T < 500ºC
High technology
Injectable conditions in the gas pipeline are achievable in Sabadell
stream H2 CH4 CO2 XCO2
% % % %
inlet 66 - 33 0
middle 30 65 10 90,85
outlet 4,4 95,4 0,2 99,77
Electric consumption SNG production Efficiency PtG XCO2
kWh Nm3/h kWh/Nm3 kWout/kWin %
Test 1 16,24 0,577 28,15 38,06 96,99
Test 2 15,84 0,536 29,58 36,13 97,75
Test 3 12,16 0,519 23,00 46,55 97,61
kWout/kWin > 50% can be
achieved within this project
85-95% power consumption comes from hydrogen production,
nevertheless surplus renewal energy production can be used.
Performant
catalysts are
the clue
Fin de semana
Intermedia
Carga
Punta
Base
Eólica
Fotovoltaica
Demanda
Solar concentración
Carga
21% RENEWABLE
SURPLUS OF ENERGY
ENERGY
CONSUMPTION
DURING A WEEK
60% renovables
WIND
ENERGY
SOLAR
ENERGY
WITHOUT
RENEWABLES
http://www.grtgaz.com/fileadmin/transition_energetique/documents/hydrogene_et_reseau_e-
cube_GRTgaz.pdf
http://www.grtgaz.com/fileadmin/engagements/documents/fr/Power-to-Gas-etude-ADEME-GRTgaz-GrDF-
complete.pdf
Source: IRES (Fraunhofer presentation) + IREC
Methanation: Solar Hydrogen +CO2
Renewable energy +feed stocks (H2, CO2)
100%
Feed stocks managements
95% Efficiency 95%; loss 5%
Methanation
76% Efficiency 80%; loss 19%
Compressor, storage and CH4 pipe
74,5% Efficiency 98,5%; loss 1.5%
Gas transport (500Km)
Efficiency 99,55%, loss 0,37%
74,1%
Methanation: Solar
Hydrogen+CO2
Dark
(or under illumination)
Carbon dioxide reduction by electrochemical (dark and photo)
procedures NEW RESEARCH
ALTERNATIVE
DARK PHOTO
Reduced
CO2 products
High current
densities
Centralizer
electrolyzer.
Current
densities of
PV cell.
Distributed
electrolyzer.
Future depends on cost
and social acceptation
Dark
Under illumination
PHOTO
EFFECT
Two challenges:
• Current density
• Bias reduction
efficient solar induced bias free working mode of a PEC cell
If curves intersect, there is enough
potential for bias free working
mode of the cell.
All that matters is the current Jop at
the intersection.
Source: several+IREC
E red E oxd
Hybrid photoanode-photocathode device for bias-free water splitting
Photoanode: Hematite, TiO2
Photocathode:
• a-Si:H tandem with Ni as HER catalyst
• a-Si:H/a-Si:H/µc-Si:H triple with Ni catalys
Electrolyte: 1M NaOH
Stability of stand-alone
hybrid Hematite/Tandem device
2-electrode config.
0 V applied biashematite
a-Si:H tandemO2
H2
To be published
Data source: F. Urbain et al. 2016&2018
System consists of two polymer electrolyte membrane electrolysers in series
with one InGaP/GaAs/GaInNAsSb triple-junction solar cell, which produces a
large-enough voltage to drive both electrolysers with no additional energy
input. The system achieves a 48-h average STH efficiency of 30%
Nat Comm 2016,7,13237
Very expensive
Use scarce
materials.
The TiO2-protected III–V tandem
device exhibited a solar-to-hydrogen
conversion efficiency, STH, of
10.5% under 1 sun illumination, with
stable performance for > 40 h
Energy Environ. Sci.,
2015, 8, 3166
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
0
5
10
15
20
IBC UPC +Ni epox + Ni/Pt PEC H2SO4
IBC UPC +Ni epox + Ni/Pt PV
HC-STH(%)
E (V vs RHE)
50cm2 area
0,650
40mA/cm2
STH >15%
PATENT:15382658.1
PEC
PV
ACS APPLIED MATERIALS & INTERFACES 10
(16) pp: 13425-13433 (2018)
Our results:
Artificial
photosynthesis:
solar refinery
Photons
Fuel
Added Value Chemicals
Solar heat
Solar electricity
H2O pipeline
CO2 pipeline
Activation Mechanisms for
H2O and CO2 reduction
Fossil fuel
power plant
Fischer Tropsch
Water
Thermo-chemical
Thermolysis
Photolysis
Photo-catalysis
CO2
Capture
Photo-electro-chemical
Electro-chemical
Solar Refinery
Chemical Storage & CO2 Circular Economy
biogenic carbon
Electrolyzers/
Co-electrolysis
.
12-20%
>10%
< 65% operation
Solar fuels
<1€/Wp
<6c€/kWh < 6c€/Kwh
photons
electrons chemicals
Data source: IREC
centralized
or
distributed
Where and how to install the
electrochemical part?
20%
19%
11%
20%
> 17%
> 17%
ELECTRICIDAD GAS
Overpotentials at several
tens of mA/cm2 ?
Overpotentials at several
tens of A/cm2 ?
Electrodes:
Voltage cell:
LHV 1,23/1,5 ~ 82%
HHV 1,48/1,5 ~ 98%
1,23/2,3 ~ 55%
Less transportation losses
Example
considering H2
PEC/EC ANODEEC CATHODE
3D
Nanostructured
Cathode
with Catalyst
Strong interest in
having back
illumination especially
for replacing
electroreduction
by
photoelectroreduction
of
CO2.
ELECTROCHIMICA ACTA
240 pp 225-230 (2017)
For CO2: Cathode with
appropriate catalyst
Anode with excellent OER.
The final energy balance as well as the
overall efficiency and productivity depend,
aside of the system design constraints, of
parameters as the over-potential values,
charge transfer resistances linked to the
role played by the catalyst.
ELECTROCHIMICA ACTA 240 pp 225-230 (2017)
PATENT: P3146EP00 PEC system for solar fuels
Carbon dioxide can give rise to different reduction reactions
pathways with several sub products. .
CO2 Reduction Products
CO2 + 2e-  •CO2
-
CO2 + 2H+ + 2e-  HCOOH
CO2 + 2H+ + 2e-  CO + H2O
CO2 + 4H+ + 4e-  HCHO+ H2O
CO2 + 6H+ + 6e-  CH3OH+ H2O
CO2 + 8H+ + 8e-  CH4 + 2H2O
2H2O + 4h+  O2 + 4H+
2H+ + 2e-  H2
CO2
Electrocatalysts reduce the overpotential of reactions through formation of
intermediates. Therefore, elucidating the intermediates is a crucial requirement
for rational design of novel catalysts that overcome the current limitations.
So, one of the objective must tackle this knowledge gap by high-risk–high-gain
approaches to prepare catalytic intermediates on oxides
CO2 reduction by metal electrocatalysis
*Source : J. Chem. SOC., Faraday Trans. I, 1989, 85(8), 2309-2326
Chem. Asian J. 2009,4, 1516-1523
 Stabilization of CO2
•–
intermediate = high
energy efficiency.
 Three groups
depending on the
binding strength
+
High HER
overpotential
CO desorption
before
reduction
+
Low HER
overpotential
HCOOH
formation
Weak CO adsorption
Strong CO
adsorption
+
Low HER
overpotential
CO poisoning
Optimum CO adsorption
CO reduction
Intermediate steps of CO2R
i.e. protonation *CHO or *COH
2
1
3
1
Gas Diffusion Electrodes
Electrolyte
Planar
Planar electrode Gas diffusion electrode
Catalyst particles
Electrolyte
CO2
chamber
GDE
• Active surface area ≈ geometric surface area
• Limited CO2 solubility = Mass transfer problem
• Active surface area >> geometric surface area
• Improved CO2 transfer = overcome solubility
problem
Toray Carbon Paper TGP-H-60 after Cu deposition
JOURNAL OF PHYSICAL CHEMISTRY C
119 ,33 , pp18835-18842 (2015)
fibers after deposition of Sn
APPLIED CATALYSIS B-ENVIRONMENTAL
150 pp 57-62 (2014)
INTERNATIONAL JOURNAL OF HYDROGEN
ENERGY 38,7, 2979-2985 (2013)
APPLIED PHYSICS LETTERS 99 ,26 ;262102 (2011)
Electrodeposited Sn in GDE
E. Irtem, J.R. Morante, et al. J. Mater. Chem. A. 2016, 4, 13582.
Dark Electrolysis
Sn catalyst  Formic acid
Dark Electrolysis
Sn catalyst  Formic acid
• F.E.% HCOO− = 71 ± 1.1 %
• F.E.% HCOO− + CO = 82 ± 2.0 % of total CO2 conversion (CO: 6 ± 4.5 %)
• Low Tafel slope value = faster charge transfer of CO2 reduction on Sn-GDE
• Evidence of a rapid transfer of the initial electron
• Evidence of a different rate determining step = concurrent proton−electron uptake
𝑭. 𝑬. % =
𝑛 · 𝐹 · [𝐶
𝐼 · 𝑡
-0.4 -0.6 -0.8 -1.0 -1.2
0
20
40
60
80
100
HCOO
CO
E (VRHE
)
FaradaicEff.(%)
H2
-2 -1 0
-0.3
-0.4
-0.5
-0.6
-0.7 H2
254 mV dec
-1
E(VRHE
)
log ji
(mAcm-2
)
-3 -2 -1 0
-0.4
-0.5
-0.6
-0.7 HCOO
89 mVdec-1
CO
78 mVdec-1
E(VRHE
)
log ji
(mAcm-2
)
E. Irtem, J.R. Morante, et al. J. Mater. Chem. A. 2016, 4, 13582.
100 1000 10000
10
100
1000activity(mol/(g*s))
grain radius (nm)
Pulsed Electro Deposition
different duty cycle
Continuous Electrodeposition
different samples
slope -1
Using other catalysts
for formic acid
submitted
JOURNAL OF MATERIALS CHEMISTRY A ,
4, 35, pp 13582-13588 (2016)
CO2 + 2e-  •CO2
-
CO2 + 2H+ + 2e-  HCOOH
CO2 + 2H+ + 2e-  CO + H2O
CO2 + 4H+ + 4e-  HCHO+ H2O
CO2 + 6H+ + 6e-  CH3OH+ H2O
CO2 + 8H+ + 8e-  CH4 + 2H2O
2H2O + 4h+  O2 + 4H+
2H+ + 2e-  H2
CO2 Reduction Products
Syngas
H2:CO ratio
3:1 Ammonia
2:1 Methanol
1:1 Oxo products
1:0 Hydrogen
...
...
...
CO2 Reduction Catalysts
Zn
J. Lee, et al. Chem. Asian J. 2009, 4, 1516-1523.
Syngas
Electrodeposition of Zn on Cu Foam
bare Cu foam 1M ZnSO4
Cu foam coated with ZnZn flakes
CE
foam
Structural Analysis of Zn Flakes
Zn
ZnO
Zn
High activity towards
CO2 reduction
Electrochemical Characterization
after 1 h electrolysis
Good stability in 0.5 M
KHCO3
F. Urbain, J.R. Morante, et al. Energy Environ. Sci. 2017, 10, 2256.
J.R. Morante et al. Energy and Environmental Science10(10), pp. 2124-2136 (2017)
5:1 ≥ H2:CO ≥
0.5:1
FEmax (CO) = 85 %
jCO = 39.4 mA/cm2
Electrochemical Characterization
F. Urbain, J.R. Morante, et al. Energy Environ. Sci. 2017, 10, 2256.
CO2 Reduction Catalysts
Zn
J. Lee, et al. Chem. Asian J. 2009, 4, 1516-1523.
Syngas
ACS applied materials and interfaces (2018)
ENERGY & ENVIRONMENTAL
SCIENCE 10 , 10, 2256 (2017)
Dark and Solar CO2 Reduction Device
Role of the anode
V
[H2(g)]
[CO(g)]
e-
h+
OH-
Na+
O2
Working Mode of Stack Flow Cell
CATHODE | CO2 reduction reaction (CO2R)
CO2 aq. +2H+
+ 2e−
⟶ HCOOH(aq.)
ANODE | H2O oxidation reaction (OER) H2O l ⟶ 2H+
+ 1
2
O2 g + 2e−
CELL REACTION 𝐂𝐎 𝟐 𝐠 + 𝐇 𝟐 𝐎 𝐥 ⟶ 𝐇𝐂𝐎𝐎𝐇(𝐚𝐪.) + 𝟏
𝟐
𝐎 𝟐 𝐠
Gas
Pure CO2
0.5 M NaHCO3
0.1 M KHCO3
0.1 M KHCO3
0.5 M KOH
0.1 M KHCO3
0.1 M KOH
Membrane
Catholyte AnolyteNafion (CEM/Na+)
Selemion (AEM/OH-)
Nafion (CEM/Na+)
Sn-GDE
Cu-GDE
Cathode
Metal oxide as
TiO2 NRs/FTO or
Other PV materials
and nanostructures
Anode
ELECTROCHIMICA ACTA
240 pp 225-230 (2017)
0,0 0,4 0,8 1,2 1,6 2,0
5
10
15
20
25
30
35currentdensityj[mA/cm2
]
0.5 m KOH
20 mV/s
potential E vs. RHE [V]
Energy Environ. Sci.,
8, 3242-3254, (2015)
ACS Appl. Mater.
Interfaces, 2016, 8, 4076
SOLAR ENERGY
MATERIALS AND
SOLAR CELLS
158 pp. 184-188 (2016)
ACS CATALYSIS 8, 4,
pp3331-3342 (2018)
JOURNAL OF
PHYSICALCHEMISTRY
C 122,6,pp 3295-3304 (2018)
ENERGY&ENVIRONMENTAL
SCIENCE 10, 10, 2124(2017)
ACS APPLIED MATERIALS&
INTERFACES 9 ,21,17932 (2017)
SOLAR ENERGY MATERIALS
AND SOLAR CELLS
159 ,456-466 (2017)
APPLIED CATALYSIS
B-ENVIRONMENTAL
189 pp133-140 (2016)
DARK
LIGHT
JOURNAL OF PHYSICS D-APPLIED PHYSICS
50 ,10, 104003 (2017)
JOURNAL OF MATERIALS CHEMISTRY A
4 ,42, pp 16706-16713 (2016)
JOURNAL OF MATERIALS CHEMISTRY A
2 ,32, pp 12708-12716 (2014)
CoFe nanoparticles are prepared by
1 mmol Iron acetylacetonate
1mmol Cobalt acetylacetonate ,
10 ml oleylamine,
1.0 ml oil acid mixed in a three-neck flask.
The solution was increased to 80 °C and
degased for 1hour. Then the temperature was
increased to 230°/ 300º with continuously
nitrogen pumping and maintained at the
selected temperature for 0.5 h.
After reaction, the received samples were
thoroughly purified by precipitation and
redispersion steps.
CHEMSUSCHEM 11, 1, pp 125-129 (2018)
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
138, 49 pp 16037-16045 (2016)
ACS APPLIED MATERIALS & INTERFACES
8, 43,pp 29461-29469 (2016)
ACS APPLIED MATERIALS & INTERFACES
8,27,pp 17435-17444 (2016)
0 2 4 6 8
20
30
40
50
60
70
80
90
100
mA
numer of dips/ mg
dips
mg
Particles size <8nm
Our
CoFe
CoFe on Ni
foam: Our
results Ƞ (EC)= 1,23/1,5= 82%
Ƞ (PV)= 23%
Ƞ total > 18,86%
10mA/cm2
Conclusions:
advances in catalysis help to
implement new technologies to
develop an eficient low cost circular
CO2 economy.
NATURE ENERGY | VOL 1 | MAY 2016 | 1-8
Research must bring
solutions to have VERY LONG
STABILITY . it IS
A KEY Issue for pec systems
and it depends on the
material developers
New materials, specially
catalysts, for Dark or Photo
electrolysis of CO2 will deploy
many new disruptive ideas in the
field of energy
Science must guide the new
energy challenges of our
society
Catalonia Institute
for
Energy Research
New call for PhD EU
program Marie Curie
https://projects.icmab.es/docfam/
jrmorante@irec.cat
Thank you.
Thanks to:
Teresa Andreu
F. Urbain
J.Arbiol
Pengyi Tan
C.Ros
N.Carretero
M. Biset

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Catalyst materials for solar refineries, synthetic fuels and procedures for a circular economy of the CO2.

  • 1. Catalyst materials for solar refineries, synthetic fuels and procedures for a circular economy of the CO2 J.R.Morante IREC, Catalonia Institute for Energy Research, Plaça de les Dones de Negre,1. Sant Adrià del Besòs, 08930. Spain. Department of Electronics, University of Barcelona, C/Martí i Franquès,1. Barcelona,08028. Spain. H2 O2
  • 2. Nowadays, the circular economy of carbon dioxide constitutes one of the major world challenges. Climatic change CO2 emissions
  • 3. The conversion of CO2 into value-added chemicals and/or fuels, using renewable energy and earth-abundant elements as well as environmental friendly materials is a key priority.
  • 4.
  • 5.  Carbon dioxide closed loop in which this molecule is captured, reduced and oxidized continuously defining an ideal circular economy of the CO2 Fossil gas CO2 emissions Methanation based on Paul Sabatier reactor.
  • 7.  Carbon dioxide reduction by thermochemical or plasma procedures which are open new alternatives to the methanation process Patent: P201530109 300mg of catalyst, corresponding to an GHSV of 20000, the reactor is supplied with a mixture of carbon dioxide and hydrogen (20% vol CO2) with a total flow rate of 12000 ml/h), at atmospheric pressure and at temperature of 20°C Journal of CO₂ Utilization 26 (2018) 202–211
  • 8. EELS chemical composition maps obtained from the red rectangled area of the STEM-HAADF micrograph. Individual Ce (red), Zr (green) and Ni (blue) maps and their composite. It should be noted here that we have normalized the intensity values of the maps to that of Ce to have a better comparison
  • 10.
  • 11. Bioconversion: Synthetic natural gas production from biogas in a waste water treatment plant In collaboration with Naturgy programa RIS3CAT ENERGY CONVERSION AND MANAGEMENT 162 pp 218-224 (2018)
  • 12. Demonstration unit [Sabadell (Barcelona) Spain) Digestor GasometerBiogas
  • 13. Methanation unit CO2 + 4H2 –> CH4 + 2H2O Alkaline electrolyzer 37 kWh Biogas source (55-65% CH4) H2S cleaning CH4 CO2 CO2 source 10 Nm3/h
  • 14. Methanation reactors Compact reactor technology Quick start-up and shut-down times Load-flexibility T depends on time, length T < 500ºC High technology
  • 15. Injectable conditions in the gas pipeline are achievable in Sabadell stream H2 CH4 CO2 XCO2 % % % % inlet 66 - 33 0 middle 30 65 10 90,85 outlet 4,4 95,4 0,2 99,77 Electric consumption SNG production Efficiency PtG XCO2 kWh Nm3/h kWh/Nm3 kWout/kWin % Test 1 16,24 0,577 28,15 38,06 96,99 Test 2 15,84 0,536 29,58 36,13 97,75 Test 3 12,16 0,519 23,00 46,55 97,61 kWout/kWin > 50% can be achieved within this project 85-95% power consumption comes from hydrogen production, nevertheless surplus renewal energy production can be used. Performant catalysts are the clue
  • 16. Fin de semana Intermedia Carga Punta Base Eólica Fotovoltaica Demanda Solar concentración Carga 21% RENEWABLE SURPLUS OF ENERGY ENERGY CONSUMPTION DURING A WEEK 60% renovables WIND ENERGY SOLAR ENERGY WITHOUT RENEWABLES
  • 18. Source: IRES (Fraunhofer presentation) + IREC
  • 19. Methanation: Solar Hydrogen +CO2 Renewable energy +feed stocks (H2, CO2) 100% Feed stocks managements 95% Efficiency 95%; loss 5% Methanation 76% Efficiency 80%; loss 19% Compressor, storage and CH4 pipe 74,5% Efficiency 98,5%; loss 1.5% Gas transport (500Km) Efficiency 99,55%, loss 0,37% 74,1% Methanation: Solar Hydrogen+CO2
  • 21. Carbon dioxide reduction by electrochemical (dark and photo) procedures NEW RESEARCH ALTERNATIVE DARK PHOTO Reduced CO2 products High current densities Centralizer electrolyzer. Current densities of PV cell. Distributed electrolyzer. Future depends on cost and social acceptation
  • 22. Dark Under illumination PHOTO EFFECT Two challenges: • Current density • Bias reduction
  • 23. efficient solar induced bias free working mode of a PEC cell If curves intersect, there is enough potential for bias free working mode of the cell. All that matters is the current Jop at the intersection. Source: several+IREC E red E oxd
  • 24. Hybrid photoanode-photocathode device for bias-free water splitting Photoanode: Hematite, TiO2 Photocathode: • a-Si:H tandem with Ni as HER catalyst • a-Si:H/a-Si:H/µc-Si:H triple with Ni catalys Electrolyte: 1M NaOH Stability of stand-alone hybrid Hematite/Tandem device 2-electrode config. 0 V applied biashematite a-Si:H tandemO2 H2 To be published
  • 25. Data source: F. Urbain et al. 2016&2018
  • 26. System consists of two polymer electrolyte membrane electrolysers in series with one InGaP/GaAs/GaInNAsSb triple-junction solar cell, which produces a large-enough voltage to drive both electrolysers with no additional energy input. The system achieves a 48-h average STH efficiency of 30% Nat Comm 2016,7,13237 Very expensive Use scarce materials.
  • 27. The TiO2-protected III–V tandem device exhibited a solar-to-hydrogen conversion efficiency, STH, of 10.5% under 1 sun illumination, with stable performance for > 40 h Energy Environ. Sci., 2015, 8, 3166
  • 28. 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0 5 10 15 20 IBC UPC +Ni epox + Ni/Pt PEC H2SO4 IBC UPC +Ni epox + Ni/Pt PV HC-STH(%) E (V vs RHE) 50cm2 area 0,650 40mA/cm2 STH >15% PATENT:15382658.1 PEC PV ACS APPLIED MATERIALS & INTERFACES 10 (16) pp: 13425-13433 (2018) Our results:
  • 30. Photons Fuel Added Value Chemicals Solar heat Solar electricity H2O pipeline CO2 pipeline Activation Mechanisms for H2O and CO2 reduction Fossil fuel power plant Fischer Tropsch Water Thermo-chemical Thermolysis Photolysis Photo-catalysis CO2 Capture Photo-electro-chemical Electro-chemical Solar Refinery Chemical Storage & CO2 Circular Economy biogenic carbon
  • 31. Electrolyzers/ Co-electrolysis . 12-20% >10% < 65% operation Solar fuels <1€/Wp <6c€/kWh < 6c€/Kwh photons electrons chemicals Data source: IREC
  • 32. centralized or distributed Where and how to install the electrochemical part? 20% 19% 11% 20% > 17% > 17%
  • 34. Overpotentials at several tens of mA/cm2 ? Overpotentials at several tens of A/cm2 ? Electrodes: Voltage cell: LHV 1,23/1,5 ~ 82% HHV 1,48/1,5 ~ 98% 1,23/2,3 ~ 55% Less transportation losses Example considering H2
  • 35. PEC/EC ANODEEC CATHODE 3D Nanostructured Cathode with Catalyst Strong interest in having back illumination especially for replacing electroreduction by photoelectroreduction of CO2. ELECTROCHIMICA ACTA 240 pp 225-230 (2017) For CO2: Cathode with appropriate catalyst Anode with excellent OER.
  • 36. The final energy balance as well as the overall efficiency and productivity depend, aside of the system design constraints, of parameters as the over-potential values, charge transfer resistances linked to the role played by the catalyst. ELECTROCHIMICA ACTA 240 pp 225-230 (2017) PATENT: P3146EP00 PEC system for solar fuels
  • 37. Carbon dioxide can give rise to different reduction reactions pathways with several sub products. . CO2 Reduction Products CO2 + 2e-  •CO2 - CO2 + 2H+ + 2e-  HCOOH CO2 + 2H+ + 2e-  CO + H2O CO2 + 4H+ + 4e-  HCHO+ H2O CO2 + 6H+ + 6e-  CH3OH+ H2O CO2 + 8H+ + 8e-  CH4 + 2H2O 2H2O + 4h+  O2 + 4H+ 2H+ + 2e-  H2
  • 38. CO2 Electrocatalysts reduce the overpotential of reactions through formation of intermediates. Therefore, elucidating the intermediates is a crucial requirement for rational design of novel catalysts that overcome the current limitations. So, one of the objective must tackle this knowledge gap by high-risk–high-gain approaches to prepare catalytic intermediates on oxides
  • 39. CO2 reduction by metal electrocatalysis *Source : J. Chem. SOC., Faraday Trans. I, 1989, 85(8), 2309-2326 Chem. Asian J. 2009,4, 1516-1523  Stabilization of CO2 •– intermediate = high energy efficiency.  Three groups depending on the binding strength + High HER overpotential CO desorption before reduction + Low HER overpotential HCOOH formation Weak CO adsorption Strong CO adsorption + Low HER overpotential CO poisoning Optimum CO adsorption CO reduction Intermediate steps of CO2R i.e. protonation *CHO or *COH 2 1 3 1
  • 40. Gas Diffusion Electrodes Electrolyte Planar Planar electrode Gas diffusion electrode Catalyst particles Electrolyte CO2 chamber GDE • Active surface area ≈ geometric surface area • Limited CO2 solubility = Mass transfer problem • Active surface area >> geometric surface area • Improved CO2 transfer = overcome solubility problem
  • 41. Toray Carbon Paper TGP-H-60 after Cu deposition JOURNAL OF PHYSICAL CHEMISTRY C 119 ,33 , pp18835-18842 (2015)
  • 42. fibers after deposition of Sn APPLIED CATALYSIS B-ENVIRONMENTAL 150 pp 57-62 (2014) INTERNATIONAL JOURNAL OF HYDROGEN ENERGY 38,7, 2979-2985 (2013) APPLIED PHYSICS LETTERS 99 ,26 ;262102 (2011)
  • 43. Electrodeposited Sn in GDE E. Irtem, J.R. Morante, et al. J. Mater. Chem. A. 2016, 4, 13582. Dark Electrolysis Sn catalyst  Formic acid
  • 44. Dark Electrolysis Sn catalyst  Formic acid • F.E.% HCOO− = 71 ± 1.1 % • F.E.% HCOO− + CO = 82 ± 2.0 % of total CO2 conversion (CO: 6 ± 4.5 %) • Low Tafel slope value = faster charge transfer of CO2 reduction on Sn-GDE • Evidence of a rapid transfer of the initial electron • Evidence of a different rate determining step = concurrent proton−electron uptake 𝑭. 𝑬. % = 𝑛 · 𝐹 · [𝐶 𝐼 · 𝑡 -0.4 -0.6 -0.8 -1.0 -1.2 0 20 40 60 80 100 HCOO CO E (VRHE ) FaradaicEff.(%) H2 -2 -1 0 -0.3 -0.4 -0.5 -0.6 -0.7 H2 254 mV dec -1 E(VRHE ) log ji (mAcm-2 ) -3 -2 -1 0 -0.4 -0.5 -0.6 -0.7 HCOO 89 mVdec-1 CO 78 mVdec-1 E(VRHE ) log ji (mAcm-2 ) E. Irtem, J.R. Morante, et al. J. Mater. Chem. A. 2016, 4, 13582.
  • 45. 100 1000 10000 10 100 1000activity(mol/(g*s)) grain radius (nm) Pulsed Electro Deposition different duty cycle Continuous Electrodeposition different samples slope -1 Using other catalysts for formic acid submitted
  • 46. JOURNAL OF MATERIALS CHEMISTRY A , 4, 35, pp 13582-13588 (2016)
  • 47. CO2 + 2e-  •CO2 - CO2 + 2H+ + 2e-  HCOOH CO2 + 2H+ + 2e-  CO + H2O CO2 + 4H+ + 4e-  HCHO+ H2O CO2 + 6H+ + 6e-  CH3OH+ H2O CO2 + 8H+ + 8e-  CH4 + 2H2O 2H2O + 4h+  O2 + 4H+ 2H+ + 2e-  H2 CO2 Reduction Products Syngas H2:CO ratio 3:1 Ammonia 2:1 Methanol 1:1 Oxo products 1:0 Hydrogen ... ... ...
  • 48. CO2 Reduction Catalysts Zn J. Lee, et al. Chem. Asian J. 2009, 4, 1516-1523. Syngas
  • 49. Electrodeposition of Zn on Cu Foam bare Cu foam 1M ZnSO4 Cu foam coated with ZnZn flakes CE foam
  • 50. Structural Analysis of Zn Flakes Zn ZnO Zn
  • 51. High activity towards CO2 reduction Electrochemical Characterization after 1 h electrolysis Good stability in 0.5 M KHCO3 F. Urbain, J.R. Morante, et al. Energy Environ. Sci. 2017, 10, 2256. J.R. Morante et al. Energy and Environmental Science10(10), pp. 2124-2136 (2017)
  • 52. 5:1 ≥ H2:CO ≥ 0.5:1 FEmax (CO) = 85 % jCO = 39.4 mA/cm2 Electrochemical Characterization F. Urbain, J.R. Morante, et al. Energy Environ. Sci. 2017, 10, 2256.
  • 53. CO2 Reduction Catalysts Zn J. Lee, et al. Chem. Asian J. 2009, 4, 1516-1523. Syngas
  • 54.
  • 55.
  • 56.
  • 57. ACS applied materials and interfaces (2018) ENERGY & ENVIRONMENTAL SCIENCE 10 , 10, 2256 (2017)
  • 58. Dark and Solar CO2 Reduction Device Role of the anode
  • 59. V [H2(g)] [CO(g)] e- h+ OH- Na+ O2 Working Mode of Stack Flow Cell CATHODE | CO2 reduction reaction (CO2R) CO2 aq. +2H+ + 2e− ⟶ HCOOH(aq.) ANODE | H2O oxidation reaction (OER) H2O l ⟶ 2H+ + 1 2 O2 g + 2e− CELL REACTION 𝐂𝐎 𝟐 𝐠 + 𝐇 𝟐 𝐎 𝐥 ⟶ 𝐇𝐂𝐎𝐎𝐇(𝐚𝐪.) + 𝟏 𝟐 𝐎 𝟐 𝐠 Gas Pure CO2 0.5 M NaHCO3 0.1 M KHCO3 0.1 M KHCO3 0.5 M KOH 0.1 M KHCO3 0.1 M KOH Membrane Catholyte AnolyteNafion (CEM/Na+) Selemion (AEM/OH-) Nafion (CEM/Na+) Sn-GDE Cu-GDE Cathode Metal oxide as TiO2 NRs/FTO or Other PV materials and nanostructures Anode ELECTROCHIMICA ACTA 240 pp 225-230 (2017)
  • 60. 0,0 0,4 0,8 1,2 1,6 2,0 5 10 15 20 25 30 35currentdensityj[mA/cm2 ] 0.5 m KOH 20 mV/s potential E vs. RHE [V] Energy Environ. Sci., 8, 3242-3254, (2015) ACS Appl. Mater. Interfaces, 2016, 8, 4076 SOLAR ENERGY MATERIALS AND SOLAR CELLS 158 pp. 184-188 (2016) ACS CATALYSIS 8, 4, pp3331-3342 (2018) JOURNAL OF PHYSICALCHEMISTRY C 122,6,pp 3295-3304 (2018) ENERGY&ENVIRONMENTAL SCIENCE 10, 10, 2124(2017) ACS APPLIED MATERIALS& INTERFACES 9 ,21,17932 (2017) SOLAR ENERGY MATERIALS AND SOLAR CELLS 159 ,456-466 (2017) APPLIED CATALYSIS B-ENVIRONMENTAL 189 pp133-140 (2016)
  • 61. DARK LIGHT JOURNAL OF PHYSICS D-APPLIED PHYSICS 50 ,10, 104003 (2017) JOURNAL OF MATERIALS CHEMISTRY A 4 ,42, pp 16706-16713 (2016) JOURNAL OF MATERIALS CHEMISTRY A 2 ,32, pp 12708-12716 (2014)
  • 62. CoFe nanoparticles are prepared by 1 mmol Iron acetylacetonate 1mmol Cobalt acetylacetonate , 10 ml oleylamine, 1.0 ml oil acid mixed in a three-neck flask. The solution was increased to 80 °C and degased for 1hour. Then the temperature was increased to 230°/ 300º with continuously nitrogen pumping and maintained at the selected temperature for 0.5 h. After reaction, the received samples were thoroughly purified by precipitation and redispersion steps. CHEMSUSCHEM 11, 1, pp 125-129 (2018) JOURNAL OF THE AMERICAN CHEMICAL SOCIETY 138, 49 pp 16037-16045 (2016) ACS APPLIED MATERIALS & INTERFACES 8, 43,pp 29461-29469 (2016) ACS APPLIED MATERIALS & INTERFACES 8,27,pp 17435-17444 (2016)
  • 63.
  • 64. 0 2 4 6 8 20 30 40 50 60 70 80 90 100 mA numer of dips/ mg dips mg Particles size <8nm
  • 66. CoFe on Ni foam: Our results Ƞ (EC)= 1,23/1,5= 82% Ƞ (PV)= 23% Ƞ total > 18,86% 10mA/cm2 Conclusions: advances in catalysis help to implement new technologies to develop an eficient low cost circular CO2 economy. NATURE ENERGY | VOL 1 | MAY 2016 | 1-8
  • 67. Research must bring solutions to have VERY LONG STABILITY . it IS A KEY Issue for pec systems and it depends on the material developers New materials, specially catalysts, for Dark or Photo electrolysis of CO2 will deploy many new disruptive ideas in the field of energy Science must guide the new energy challenges of our society
  • 68. Catalonia Institute for Energy Research New call for PhD EU program Marie Curie https://projects.icmab.es/docfam/ jrmorante@irec.cat
  • 69. Thank you. Thanks to: Teresa Andreu F. Urbain J.Arbiol Pengyi Tan C.Ros N.Carretero M. Biset