STABLE Description WP3LEITAT– January ,2013

Synthesis and optimization of electrolyte of Li-air cells

David AmantiaChristophe Aucher

LEITAT

STABLE WP3 organizationJanuary, 2013

STABLE Description WP3LEITAT– 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

Participant id

POLITO

LEITAT

LUREDERRA

IVF UCCSA

U

CEGASA

ELAPHE

 

Person-months per beneficiary:

14 20 6 0 0 8 6 2 

Start date or starting event: M1End date: M32

STABLE Description WP3LEITAT– January ,2013

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 WP3LEITAT– 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 quantityOxygen & by-product solubility ↑Water content ↓, Hydrophobicity ↑Electrochemical windows ↑Stability (cycling) ↑Safety ↑

STABLE Description WP3LEITAT– January ,2013

Filling amount

Objective

Commercial solution

Price

WatercontentConduc

tivity

Viscosity

Oxygen solubility

Stability

By- product

solubilitySolvent Evaporation -E

Safety

NewElectrolyte

Bibliographic surveyMost 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?

CandidatesPhysical and chemical characterizationThere is an interest to not use a commercial solution ?

Candidates

ElectrochemicalcharacterizationFinal confrontation between commercial and innovative solution (performances)

yes yes

NoNo

STABLE Description WP3LEITAT– January ,2013

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 WP3LEITAT– January ,2013

Organization (proposition)

Task 3

.3Ta

sk 3

.2Ta

sk 3

.1 PC/DEC/EC

RTILs(melts preparation)

Additives1) electrolyte2) LISICON modification

Additives

RTILs (characterization)

Database

Repport(template proposed: (1)State of the art SoA, (2) Beyond SoA, (3) Table comparative)All technical data (numbers), Price, Safety, Other…

Synthese & Physical/ChemicalCharacterizations Battery

Sampleswater content, purity (ions contents), conductivity, thermal properties (volatility, degradation, Mp, Bp…), O2 solubility, viscosity, Other…

Samples-Up scalingElectrochemical windows, Capacity, EIS, rate of charge/discharge, energy & power density, Stability (cycling), By-product solubility, Filling amount, gas (nature, flow), Price, SEI, Other…

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…)

Lab scale

Cegasa, Polito, Leitat

?

Input(Material, production, Power&Energy needs…)

M2

4

M7

M1

2

M1

2

M1

2M7

M7

M7

EVLab scale M24

Sam

ple

s tr

ansf

ert

Feed

back

?

STABLE Description WP3LEITAT– January ,2013

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 physicalconditions for electrolyte. [month 32]

STABLE Description WP3LEITAT– January ,2013

Deliverables Information available from page 6 to 51 of Annex I

Title Description Date

D1.1 Electrolyte solvent synthesis and optimization (I): Report on description of preparation and characterizationof 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.

M12

STABLE Description WP3LEITAT– January ,2013

Proposed deadlines

M7 – April 2013: Reports (SaO, specifications, parameters...)First synthesis or melts preparationFirst characterizations (chemical, physical)

M24 – septembre 2014: First pack cells

M12 – September 2013: First complete experimental specifications(e.g. All: chemical, physical and electrochemical tests)

STABLE Description WP3LEITAT– January ,2013

Thank you for your attention

STABLE Description WP3LEITAT– January ,2013

Synthesis and optimization of electrolyte of Li-air cells

Le

itat

Toolb

ox

Designation Utility EquipmentGlove box Rate of O2 and H2O > 0.1 ppm

1) Preparation of the electrolyte (i.e. salt of lithium+ solvent.)2) Assembly of the electrochemical cell3) Electrochemical test inside the glove box (Electrolyte electrochemical Windows)

Glove Box UNILAB (4 gloves)

IC Ionic ChromatographyCl-, BF4

-, TFSI-, TFO-, PF6-, NO3

-, CH3COO-, NH3-…

(detection limit = 0,1 ppm – 10 ppm)

Dionnex ics 300Sample charger As-DV

Karl Fisher High precision for the determination of the water content.10 – 1000 µg, ± 3 µg

Coulometer KF 831

Potentiostat / Galvanostat

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.

VMP3Autolab

TGA Thermal Gravimetric AnalyzeConventional method for determining the temperature of the degradation of the solvent and the water content.

TGA Q500

DSC Differential Scanning CalorimeterConventional method for determining the physical properties of the solvent (melting, freezing points…)

DSC Q20

FTIR Fourier Transform InfraRed spectrophotometerConventional method for determining the nature of the different bonds.

IRAffinity-1

Conductimeter Conventional method for determining the conductivity of the solvent and electrolyte. Possibility for checking the conductivity at different temperature.

Ec-Meter Basic 30+Titanium cell for viscous liquid and Platinum cell for conventional liquid.

Viscosimeter Conventional method for determining the viscosity of the solvent and electrolyte. Possibility for checking the viscosity at different temperature.

Brookfield LVDV-E VicometerLV spindle set (from 61 to 64)