Synthesis and optimization of
electrolyte of Li-air cells
STABLE WP3 organization
January, 2013
David Amantia
Christophe Aucher
LEITAT
STABLE Description WP3
LEITAT– January ,2013
Overview Information available from
page 6 to 51 of
Annex I
Work package number
WP 3
Start date or starting
event:
M32
Work package title
Synthesis and optimization of electrolyte of Li-air cells
Activity Type
RTD
LEITAT
LUREDERRA
IVF
UCC
SAU
CEGASA
ELAPHE
Person-months per
beneficiary:
POLITO
Participant id
14
20
6
0
0
8
6
2
Start date or starting event:
End date:
STABLE Description WP3
LEITAT– January ,2013
M1
M32
Overall goals Information available
from page 6 to 51 of Annex I
Objectives
 - Synthesis and characterization of stable electrolyte with low
viscosity and high oxygen solubility to increase the discharge
current density.
 Synthesis, characterization and evaluation of the
performance of the electrolyte with different additives in
terms of their effect to volatility, viscosity and conductivity of
electrolyte.
 - Determination of the most suitable lithium air battery
materials and technology for the use in EVs.
STABLE Description WP3
LEITAT– January ,2013
Objective
Work will be focused on:
-the
preparation/characterization of IL/solvent/additives/salt melts
-studies on SEI
-Optimization
of PC/EC/DEC/DMC melts
-Build new ILs by ions exchange from conventional RTILs or other precursors.
-Additives for by-products and oxygen solubility
Challenge = reach the best ratio between:
Conductivity
(& viscosity, temperature) ↑
Solvent evaporation ↓
Electrolyte quantity
Oxygen & by-product solubility ↑
Water content ↓, Hydrophobicity ↑
Electrochemical windows ↑
Stability (cycling) ↑
Safety ↑
STABLE Description WP3
LEITAT– January ,2013
Objective
Commercial
solution
New
Electrolyte
Byproduct
solubility
Filling
amount
Solvent
Evapor
ation
Safety
Most of these parameters
could be evaluated by a
simple survey of the previous
works or by comparison of
the technical data sheets for
the commercial products. Will
we be able to upscale the
quantity?
yes
Candidates
No
E
Viscosity
Stability
Conduc
tivity
Bibliographic survey
Oxygen
solubility
Water
content
Price
Physical and
chemical
characterization
yes
Candidates
There is an interest to
not use a commercial
solution ?
STABLE Description WP3
LEITAT– January ,2013
No
Electrochemical
characterization
Final confrontation between
commercial and innovative
solution (performances)
Workplan Information available from
page 6 to 51
of Annex I



Task 3.1: Synthesis and optimization of room temperature ionic
liquids (RTILs) or combinations solvents properties for the aim of
obtaining good performance electrolyte solvents (Month 1- Month
32, POLITO (14 MM), LEITAT (12 MM) and CEG (6 MM)).
Task 3.2: Investigation on influence of aprotic additives to RTILs on
properties and oxygen solubility etc. (Month1- Month 32, 8MM,
SAU).
Task 3.3: Investigation and evaluation of physical properties of
RTILs and the optimum filling amount of electrolyte. Material and
production techniques analysis including LCA (Month 1- Month 32,
LEITAT (8MM), LUREDERRA (6MM), Elaphe (2MM))
Milestones (M7, M8, M9)
Deliverables (D3.1, D3.2, D3.3)
STABLE Description WP3
LEITAT– January ,2013
Organization (proposition)
Melts Preparation.
To complete a database by studying always the same parameters. Exchange between partners
to lead to the complete evaluation of the samples depending of the skill/equipment availabilities.
(dry/glove box, potentiostat, karl fisher, ionic chromatography, reference cell, cell pack…)
Database
Synthese & Physical/Chemical
Characterizations
Battery
EV
1) electrolyte
2) LISICON modification
M12
M7
M7
Additives
?
?
Lab scale
M12
RTILs
M24
Cegasa, Polito, Leitat
(melts preparation)
Task 3.2
M24
PC/DEC/EC
M12
Task 3.1
Lab scale
(characterization)
M7
RTILs
M7
Task 3.3
Feedback
Samples transfert
Additives
Input
(Material, production,
Power&Energy
needs…)
Repport
(template proposed: (1)
State of the art SoA, (2)
Beyond SoA, (3) Table
comparative)
All technical data
(numbers), Price, Safety,
Other…
Samples
Electrochemical windows, Capacity,
EIS, rate of charge/discharge,
energy & power density, Stability
(cycling), By-product solubility,
WP3
Filling amount, gas (nature, flow),
Price, SEI, Other…
,2013
water content, purity (ions contents),
conductivity, thermal properties
(volatility, degradation, Mp, Bp…), O2
solubility, viscosity,
Other…
STABLE
Description
LEITAT– January
SamplesUp scaling
Deliverables Information available from
page 6 to 51
of Annex I
D3.1) Electrolyte solvent synthesis and optimization (I): Report on description of preparation and
characterization of lithium air battery electrolytes: 1) Preparation and characterization of salt and
different compositions of ionic liquids with physical and chemical specifications; 2) Preparation and
characterization of suitable additives or fillers to RTILs; 3) Investigation of suitable conditions for
electrolyte such as filling amount and environment impact specifications such as temperature and
pressure etc. [month 12]
D3.2) Electrolyte solvent synthesis and optimization (II): Report on description of improvement on
performance of produced lithium air battery electrolytes: 1) Optimization of the physical properties
and electrochemical performance of the produced electrolytes such as viscosity and ion conductivity
through adding suitable additives. Electrolyte will be analyzed by Raman spectroscopy after
subjecting the anode to the electrolyte with different times, oxygen solubility will also be tested; 2)
Optimization of the salt and different compositions for ionic liquids; 3) Determination of suitable
conditions for electrolyte such as filling amount and environment impact specifications such as
temperature and pressure etc. [month 24]
D3.3) Conclusion on electrolyte solvent synthesis and optimization: Report on description of
assessment on the prepared electrolytes in terms of physical and electrochemical performances: 1)
Selection of optimum additives for electrolyte; 2) Selection of optimum electrolyte compositions
with good physical specification (i.e. conductivity versus temperature, electrochemical windows,
viscosity versus temperature); 3) Obtaining the optimum physical
conditions for electrolyte. [month 32]
STABLE Description WP3
LEITAT– January ,2013
Deliverables Information available from
page 6 to 51
of Annex I
D1.1
Title
Description
Date
Electrolyte solvent
synthesis and
optimization (I):
Report on
description of
preparation and
characterization
of lithium air
battery
electrolytes:
1) Preparation and characterization of
salt and different compositions of ionic
liquids with physical and chemical
specifications
M12
2) Preparation and characterization of
suitable additives or fillers to RTILs
3) Investigation of suitable conditions
for electrolyte such as filling amount
and environment impact specifications
such as temperature and pressure etc.
STABLE Description WP3
LEITAT– January ,2013
Proposed deadlines
M7 – April 2013:
Reports (SaO, specifications, parameters...)
First synthesis or melts preparation
First characterizations (chemical, physical)
M12 – September 2013:
First complete experimental specifications
(e.g. All: chemical, physical and electrochemical tests)
M24 – septembre 2014:
First pack cells
STABLE Description WP3
LEITAT– January ,2013
Thank you for your attention
STABLE Description WP3
LEITAT– January ,2013
Synthesis and optimization of electrolyte of Li-air cells
Designation
Glove box
IC
Potentiostat /
Galvanostat
TGA
DSC
FTIR
Conductimeter

Leitat Toolbox
Karl Fisher
Viscosimeter
Utility
Rate of O2 and H2O > 0.1 ppm
1) Preparation of the electrolyte (i.e. salt of lithium+ solvent.)
2) Assembly of the electrochemical cell
3) Electrochemical test inside the glove box (Electrolyte electrochemical
Windows)
Ionic Chromatography
Cl-, BF4-, TFSI-, TFO-, PF6-, NO3-, CH3COO-, NH3-…
(detection limit = 0,1 ppm – 10 ppm)
Equipment
Glove Box UNILAB (4 gloves)
High precision for the determination of the water content.
10 – 1000 µg, ± 3 µg
2 potentiostat / galvanostat are available for testing, (1) electrolyte
(conductivity, O2 reduction, potentials windows) and (2) complete cell in a
Swagelok system where the purity and gas pressure could be controlled.
Coulometer KF 831
Dionnex ics 300
Sample charger As-DV
VMP3
Autolab
Thermal Gravimetric Analyze
TGA Q500
Conventional method for determining the temperature of the degradation
of the solvent and the water content.
Differential Scanning Calorimeter
DSC Q20
Conventional method for determining the physical properties of the solvent
(melting, freezing points…)
Fourier Transform InfraRed spectrophotometer
IRAffinity-1
Conventional method for determining the nature of the different bonds.
Conventional method for determining the conductivity of the solvent and
electrolyte. Possibility for checking the conductivity at different
temperature.
Conventional method for determining the viscosity of the solvent and
electrolyte. Possibility for checking the viscosity at different temperature.
STABLE Description WP3
LEITAT– January ,2013
Ec-Meter Basic 30+
Titanium cell for viscous liquid and Platinum cell
for conventional liquid.
Brookfield LV
DV-E Vicometer
LV spindle set (from 61 to 64)