prof. linda nazar at basf science symposium 2015
TRANSCRIPT
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Ludwigshafen, Germany
BASF 150th Anniversary Symposium
Amiens
NEW VISTAS IN ELECTROCHEMICAL ENERGY
STORAGE
March 9, 2015
Prof. Linda Nazar, FRSC
Senior Canada Research Chair
Electrochemical Energy Materials Laboratory
BASF International Scientific Network for Electrochemistry and Batteries
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• Power consumption worldwide 2012: ~17 terawatts -> 28 terawatts by 2050
currently ~ 85% from the combustion of fossil fuels
• Solar: 23,000 TWy/yearlow percentage of renewable energy in global energy portfolio
Urban pollution, CO2 emissions → climate change
Finding Sustainable Energy Solutions
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• potential flood regions, Boston
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Electrochemical energy storage: a key enabler
EV ↔ Grid
EV ↔ Home
Storage ↔ Grid
Off-peak capture essential
More important today than at any time in history: new large-scale demands
Future Na-ion
Ultracapacitors
Na/Li sulfur
Redox flow
Li-ion
Li sulfur/air
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Electrochemical Energy Science– past and future
Outline
Storing electrons and ions:- Intercalation chemistry
Storing electrons and ions:- Chemical transformations
Li-Sulfur and Li-Air cells
Conclusions
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Waterloo Institute for Nanotechnology and the
Quantum-Nano Centre
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Rechargeable Li-ion Cells: Intercalation Batteries
in·ter·ca·lateinˈtərkəˌlāt/verb1. interpolate (an intercalary period) in a calendar.2. insert (something) between layers in a crystal lattice, geological formation, or other structure.
Capacity: Electrons stored per mass (mAh/g)
or volume (mAh/L)
Light weight/dense
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LiMO2 ↔ Li+ + electron + Li1-xMO2 (M= Ni, Mn,Co)
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1990 Intercalation Batteries: Chemistry Between the Sheets!
positive electrode: specific capacity around 180 mA•h/g @ voltage 3.9 V
Li-ion Storage in a Typical Electric Car Battery
700 Wh/kg (+ ve)
200 Wh/kg (full cell)
(electrons)
+
-
110 Wh/kg (pack)
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2014 Draper Prize in Engineering for Li-ion Batteries
John Goodenough pictured with fellow Draper Prize recipients Akira Yoshino, Yoshio Nishi and Rachid Yazami at the award reception in February, 2014.
John Goodenough Wins Engineering’s Highest Honor for Pioneering Lithium-Ion Battery
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• Poor accessibility of the world’s largest lithium reserves• remote locations• political factors (new Li sources: Bolivia; Afghanistan)
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vs
0.3V penalty vs Li; higher mass Greater volume change on during cycling
• Popular in the 80’s (before mobile tech)L.F. Nazar et al., Below Lithium-Ion: The Emerging Chemistry of Na-ion Batteries for Electrochemical Energy Storage, Angewandte Chemie, 2015
Below Li-ion: Coupling to Renewable Energy
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Below Li-ion: Sodium Metal Layered Oxides and Phosphates
Ellis, Nazar et al., Nature Mater., 6, 749 (2007);
Discharged(reduced)Na2FePO4F
Charged(oxidized)NaFePO4F
-Na+/e-Langrock et al., J.P.S., 223, 62 (2013)
Figure 1. Schematic presentation of the P2-
NaxMO2 crystal structure
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Na2FePO4F
Na+Li+
0.36 eV, 2-D ion transport
Activation energy for Na+ mobility lower than in many Li-ion metal phosphates
Activation barrier: 0.67 eV 1-D ion transport
Comparisons of alkali-ion mobility
LiFePO4
Tripathi, Gardiner, Islam, Nazar. Energy. Environ. Sci., 6, 2257 (2013)
→ Na+ diffusion coefficient : equal to LiCoO2
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High Voltage Na-ion Batteries : Na4NiP2O7F2
Voltage: ~ 5V2160 Wh/L (+ ve)
5V vs Na → suitable negative electrode, electrolyte → high power
~ 600 Wh/L full cell
Measured: Ea = 0.32 eV
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Computation
Kundu, Tripathi, Nazar, Chem Mater, 2015
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Enroute to a Solid State Battery
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From MRS Bulletin, Dec 2014:Solid State Batteries enter EV FrayToyota roadmap suggests all solid-state batteries are an important step in the evolution of batteries for electric vehicles, but are not the ultimate solution. Figure courtesy of H. Iba (Toyota Motor Corporation)
Schematic of an all-solid state battery
Na4NiP2O7F2
NaSICON
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Source: P.G. Bruce et al., Nature Mater., 11, 19 (2012)
Gasoline: 12000 Wh/kg
Source: P.G. Bruce et al., Nature Mater., 11, 19 (2012)
not much has changed: not true!
no Moore’s law (# transistors on an IC doubles every 2 years): true!
Misconceptions About Energy Storage Batteries
Higher energy density - better EV range at lower cost - reduced dependence on fossil fuels - less CO2 emission
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25% efficient
> 90% efficient
"storage" via low-cost intercalation chemistry is limited
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Potential Generation 3 (or 4) Batteries: Lithium-Sulfur; Lithium-Oxygen
Beyond Li-ion Intercalation: Chemical Transformations
oxygen
Li-O2 Batteryproduct: Li2O2
stored in host cathode
O2 + 2 Li+/e- ↔ Li2O2
Theoretical: 3500 Wh/kgPractical: ~ 1000 Wh/kg
H+
oxygen
Li-S Batteryproduct: Li2Sstored in host cathode
S2 + 4 Li+/e- ↔ 2Li2S
Theoretical: 2500 Wh/kgPractical: ~ 600 Wh/kg
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Resources of elemental sulfur (volcanic deposits, sulfur associated with natural gas, petroleum, tar sands, and metal sulfides: about 5 billion tons.
http://minerals.usgs.gov
$170/ton
Sulfur: a low cost, abundant element
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Canada is the world’s largest exporter of sulfur
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Lit
hiu
m
Se
pa
rato
r
Li+
2 Li+
Li+Li2S8
a(Li2S6) + b(Li2S4)
(Li2S)
e-e-
Discharge
—maintain active mass? Li2S
Li2Sx Li2Sx/2
Charge Polysulfide shuttle
internal “short circuit”
2Li + S Li2Sx Li2S theoretical capacity 1675 mAh/g @ 2V
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Beyond Li-ion Intercalation: The Li-S Battery
2500 Wh/kg (full cell)500 - 1000 mAh/g today
-> 350 Wh/kg
Lit
hiu
m
cheese milk cheese
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Space is precisely tuned to accommodate swelling of S to Li2S
Electrical Conductivity: sulfur: negligiblecarbon/sulfur: 0.21 S/cm
Mesoporous carbon
Molten S within pores( incomplete Filling)
C/S – 70 wt%
Li2S formed in close electrical contact with carbon - enables recharge
Solidification
D. Ji, K T Lee, L.F. Nazar, Nature Mater., 8, 500 (2009)
Cathode: S (elemental) + 4 Li+ + 4 e- ↔ 2Li2S Anode: 4Li ↔ 4Li+ + 4e-
Revitalization of Li-S Battery Chemistry
How Li-S battery chemistry works
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Bimodal nanostructured carbon cathode hosts - Li-S cells
Schuster, He, Bein, Nazar; Angew Chemie, (2012)He, Schuster, Mandelbrot, Bein, Nazar, Chem. Mater (2014)He, Nazar; ACS Nano (2013)Cuisinier, Balasubramanian, Nazar, J. Phys. Chem Lett (2014)Cuisinier, Balasubramanian, Nazar, Adv. Energ. Mater (2014)
For 1000 mAh/g capacity:
1400 Wh/kg based on total mass of cathode (S + carbon + binder)
2330 Wh/l volumetric for cathode
600 – 800 Wh/kg for a full cell
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In situ cell: synchrotron
0 20 40 60 80 1000
200
400
600
800
1000
1200
1400
1600
Co
ulu
mb
ic E
ffic
ien
cy (
%)
Cap
acit
y (m
Ah
/g)
Cycle Number
0
20
40
60
80
100
C/20
C/5
C/2 1C
Stable cycling
Bimodal nanostructured carbon cathode hosts - Li-S cells
Discharge/charge in 5 hours
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The Problem with Carbon Good interaction with sulfur
No interaction with lithium polysulfides OR Li2S
Li
Charge- +
Li X / solventLi2S
Shuttle MechanismLi
Discharge
Self discharge
X
LiX/ solvent
Li2Sn (polysulfide) intermediates:
Soluble in the electrolyte physical entrapment not sufficient
Sulfur
The Problem with Porous Carbon
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Cuisinier, Balasubramanian, Nazar, J. Phys. Chem Lett (2014)
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Tailoring the Surface Interaction: Oxides
Yi Cui et al., Nature Commun., 4, 1331, 2012
Q. Pang, L.F. Nazar, et al., Nature Comm., 5:4759, 2014
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Ti4O7
Metallic Ti4O7 : 2-in-1 host
Half the capacity fade rate compared to carbon
High electronic conductivity delivers electrons to S and Li2S High surface area and pore volume bind sulfur/polysulfide Surface properties inhibit polysulfide diffusion into the electrolyte
Insulating SiO2 or TiO2
L.F Nazar et al., Nature Commun., 2:325, 2011; J. Phys. Chem.
C., 116, 19653 (2012); Adv. Energ. Mater., 2, 1490 (2012)
Conductive VOx
X.Y Tao, W.K. Zhang, Yi. Cui, et al., Nano Lett., 14, 5288, 2014
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Bifunctional polysulfide sponges: High electronic conductivity (metallic) hydrophilic nature for binding lithium polysulfides
Ti4O7 crystals
carbon
200 nm
Nanocrystalline (10 -20 nm)
Ti4O7 - a metallic oxide with a hydrophilic surface
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During discharge: Much lower fraction of polysulfides at all stages (efficient trapping) Li2S precipitates earlier and more progressively
Solid: Ti4O7/SDash: C/S
Ti4O7-polysulfide interaction promotes charge transfer
Operando XANES: Ti4O7/S cathode shows strong interaction
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Ti-Ox e- e- e- e-
S8 Li2Sx2-
Ti4O7
e- e-
Solvated Li+
“adsorbed” Li2S
e-
Sulfur reduces and adsorbs on metallic oxide surface → “adsorbed” Li2S
Sulfur reduced and dissolves to form solvated lithium polysulfides→ Li2S isolated from electron wiring
Carbon e- e- e- e-
S8
Solvated Li+
Li2Sx2-
Carbon
“disconnected”Li2S
disproportionationUpon electrochemical reduction (receiving e- and Li+):
• Uniform deposition of Li2S• Suppress polysulfide diffusion/shuttle• Improved capacity retention
Q. Pang, D. Kundu, M. Cuisinier, L. F. Nazar, Nature Comm, 5 : 4759 (2014)
Ti4O7 - surface enhanced electrochemistry
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Tuning the Sulfur-Host Interaction: Functional Layered Materials
X. Liang, L.F. Nazar, et al., Nature Comm., 5:5682, 2015
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δ-MnO2
Mn3+ Mn2+Mn3+ Mn2+
catenate
Longevity (> 1500 cycles) now attainableTailor surface properties to bind (poly)sulfide
Y. Qiu, Y. Zhang, et al., Nano. Lett., 4827, 2014
- graphene oxide- N-doped graphene
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MnO2 nanosheet sulphur hosts: accomodate high sulfur loading
δ MnO2– birnessite – nanosheets 10 nm thin
100nm
75 wt % sulfur/ “inorganic graphene”
melt diffuse sulphur =>
S map Mn map
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Glass cell: Visual evidence of polysulfide trapping by MnO2
Comparison with sulfur/carbon electrode with same sulfur loading
S/KB cell
S/MnO2 nanosheet cell
0 hr 0.5 hr 4 hr 8 hr 12
hr
Almost colorless solution for S/MnO2 electrode at point of max LiPS formation
Interaction between MnO2 and polysulfide
B. Catenation of sulfur to form polythionate complex
A. Formation of thiosulfate via oxidation of LiPS/ reduction of Mn4+:
S/KB cell
S/MnO2 nanosheet cell
0 hr 0.5 hr 4 hr 8 hr 12 hr
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Interaction between polysulfide and MnO2 or graphene oxide
Li2S4
Li2S4/MnO2
Li2S4/Grapheneoxide
Li2S4/Graphene
At 2.3 V: partial reduction or oxidation
Li-S/MnO2 cell cathodeSB (0)
ST (-1)
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Polysulfide Adsorptivity of Sulfur Hosts
• Non-polar materials (carbons) adsorb much less Sn2- compared to
polar materials (metallic oxides etc)
C. Hart, M. Cuisinier, L. Nazar et al. Chem Comm, 2015, DOI: 10.1039/C4CC08980D
Electroanalytical determination of residual polysulfide
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0 40 80 120 160 2000
200
400
600
800
1000
1200
1400
1600
Cap
ac
ity (
mA
h g
-1)
Cycle number
MnO2 nanosheets: long term cycling
Capacity fade rate = 0.04% per cycle over 2000 cycles
Equivalent to some“conventional” lithium metal oxide cells
Challenge remains: sulfur loading & Li negative electrode
X. Liang, A. Garsuch, T. Weiss, L.F. Nazar*, Nature Commun., 5:5682, 2015
Cycling in 5 hours
vv
0 200 400 600 800 1000 1200 1400 16000
200
400
600
800
1000
1200
1400
1600
Charge
Discharge
Ca
pa
cit
y (
mA
h g
-1)
Cycle number
C/2
Cycling in 2 hours….over 2/3 year
In collaboration with BASF
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A Roadmap for Li-S cell design
all solid state batteries
sulfur/polysulfides
chemical confinementstrong interactions of sulfides with conductive host
highly solvating
electrolytes
“Catholyte” cells*redox flow
Nazar, et al.,
Adv Energy Mater, 2015
non-solvent
electrolytes
*high capacity*interface challenges
Nazar, et al.,
Energy Environ Sci, 2014
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Looking to the future
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All-solid-state batteries (Li, Na, Li-S, etc) have in common with Lithium-air the requirement of strict control of interfaces
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O2 + 2 Li+/e- ↔ 2 LiO2 → Li2O2 + O2
Many challenges in the Li-O2 cell
Eo = 2.96 V
2
2.5
3
3.5
4
4.5
5
0 500 1000 1500 2000 2500 3000
Po
ten
tia
l /
V
Capacity / mAh g-1
Δηa
ΔEOCP
Electrolyte reactivity
carbon
Poor round trip efficiency; poor cycling; sensitivity to CO2…
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Reactivity of the intermediate (equivalent to polysulfides) Need robust surface and electrolyte
Reactivity of the electrolyte with peroxide on charge Need a better electrolyte!
Reaction of lithium peroxide with carbon on charge C + Li2O2 + ½ O2 Li2CO3
Need a metallic, nanoporous, non-carbon catalytic surface
Many challenges in the Li-O2 cell
O2 + 2 Li+/e- ↔ 2 LiO2 → Li2O2 + O2
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Significant progress on cathode supports..
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Nanostructured Ti4O7: Metallic Oxide Cathode Host
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Electrochemistry of a metallic Magnéli-phase Ti4O7 cathode in a Li-O2 cell onset of oxygen evolution at equilibrium potential (2.96 V vs Li/Li+)
D. Kundu, R. Black, B. Adams, Energy & Environ. Science, 2015
Ti4O7
On-line mass spectrometry: gas evolution during charge of a Li-O2 cell
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Energy storage: one component of energy management
Battery materials/electrochemistry is remarkably multifaceted▪ Complex chemistry at both electrodes; in electrolyte/at interfaces▪ Sophisticated in-situ methods developed to peer into working cells
Not one energy storage battery that fits all needs ▪ transportation
- Li-ion; future: Li-S; Li-O2 (?)▪ grid/mini-grid
- Na-ion (non-aqueous, aqueous); Na-O2, Mg-ion
Energy management needed for the next decade: combination of▪ energy conversion (photovoltaics, solar fuels..)▪ energy storage ▪ energy efficiency via electrochromic windows, LED lighting, software control…
Infrastructure (smart grids) to network the system
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Brian Adams
Thank You!
BASF International Scientific Network for Electrochemistry and Batteries
Prof. M. Wagemaker, TU Delft (Netherlands)Dr. Mali Balasubramanian, Argonne NL, USA
Prof. M. Saiful Islam, Univ Bath, UKProf. T. Bein, LMU Munich, Germany
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THANKS TO:
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Happy 150th Anniversary BASF! ….from Waterloo Institute of Nanotech
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