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  • AMELIE : Advanced Fluorinated Materials for High Safety, Energy and Calendar Life

    Li Ion Batteries

    European Green Car Initiative 3d European Green Car Initiative Project clustering Event

    July 11 & 12 2012Th BAERT

  • Outline

    AMELIEs new Materials in Li ion Battery.

    Motivation, objectives, key Milestones

    Key progresses at Mid terms

    The electrodes.

    The interaction new Electrolyte / new Separator

    Eco-design, Recycling and LCA.

    Partial Conclusions

  • Project general information

    Project full title: Advanced Fluorinated Materials for High Safety, Energy and Calendar Life Li Ion Batteries.

    Coordinator contacts: Thierry.Baert@Solvay .comStarting Date: 01 Jan 2011Ending Date: 01 Jan 2014

    Budget Total/Funding: 5,2 MEUR / 3,5 MEURPartners:

  • Motivation and objectives.

    Focus on an increased autonomy of EV/PHEV with improved safety of the

    battery and cost controlled improved by recycling of some higher value

    materials.

    Research needs towards develop of a higher specific energy cell with a high voltage cathode material, and the corresponding stable electrolyte

    (solvent and Salt) with new separators, binders and extended recycling

    process

    Approach based on a new electrolytes will be based on fluorinated solvents, Sulfonimide salts, specific additives to decrease the fading,

    combined with fluorinated polymers as binders, and components of new

    separator

  • Specifications of the final deliverable.

    0

    20

    40

    60

    80

    100

    Energy

    Power

    Calendar Life

    PriceCycle Life 80DoD

    Operating Temperature

    Recyclability/ Reuse

    2010

    Project Target

    2015

    >200 Wh/kg in a 12,5 Ah Primatic wounded soft package cell

    650 W/kg, 50% SOC, 2C

    Self discharge : < 5%/ month at 25 Cand < 10% at 45 C

    80% Capacity remaining @ >1000 cycles

    and within V limits at 25 C (100% DoD,1C, Vlimit)

    + 5 Safety test : mechanical, thermal (130 C), and 3 electrical.

  • Motivation / objectives / milestones

    During the 1st Half of the project, mainly developments at lab scales are performed.

    Testing of 2 to 4 Pilot 2 Ah iterations will be running during the 2d half.End of 2013 the final cell will be scale-up to 12,5Ah.

    End 2012 the electrolyte and separator solution will be implemented in this cell.

    At mid term (July 2012) the scale-up jobs (first up to 2,5 Ah cell) will be starting by the production of electrodes.

    2011 2012 2013

    General Milestones plan.

    Cells testing at Lab level

  • Key Progress in 2011

    The High Voltage cathode material has been selected as LNMO. The adequate volume for testing have been produced at CEA.

    During the 1st Half of the project, mainly developments at lab scales are performed.

    Testing of 2 to 4 Pilot iterations will be running during the 2d half.End of 2013 the final cell will be scale-up to 12,5Ah.

    2011 2012 2013

    Developments of new (PVDF based )polymers as binders and for separator

    The formulation of cathode and anode have been design including namely the binder selection. Some fine tuning will be done during the scale-up phase.

    Developments of new additives for the Cathode

    Cells testing at Lab level

  • Key progress in 2012

    During the 1st Half of the project, mainly developments at lab scales are performed.

    Testing of 2 to 4 Pilot iterations will be running during the 2d half.End of 2013 the final cell will be scale-up to 12,5Ah.

    2011 2012 2013

    Prototype cells have been compared to our references cells (Commercial 18650 cell and own electrodes produced with commercial NMC ref material), testing the new electrodes.

    5 different salts have been designed and produced. A preliminary screening of performances lead to select 2 of them that are under testing regarding their compatibility with the new solvents (going to binary mixtures), new additives, and the polymer selected for the separator.

    New polymers for separators tested with different reinforcement technologies.

    Cells testing at Lab level

  • Main technical activities - on Electrodes

    The high Voltage cathode material (LNMO

    4,9 V) has reached the scale-up phase.

    A low content PVDF binder has been

    selected.

    The Anode has been formulated with a

    selection of Graphite, CB and with

    different type of PVDF binders.

    The most adapted formulation has been

    selected.

    The slurry properties have been studied

    as well, to optimize the coating production

    process.

  • Main technical activities - on Electrolyte/Separators

    The interaction new Electrolyte / new PVDF Separator have been tested in

    different configuration.

    Major improvements of the mechanicalproperties have been obtained and give

    access to thinner membranes, lower

    impedance.

    The production process at lab level still remain challenging to tune and to control

    avg pore size and their size distribution

    repartition, especially when reinforced.

  • Main technical activities - on Separator

    Membranes have been cycled in cell with accepable results, but the thickness need to be reduced down to 20m or lower.

    1

    10

    100

    1000

    10000

    -30 0 30 60 90 120 150 180

    Storage

    modulus

    (MPa)

    T (C)

    effect of NCC addition on dry

    membranes

    composite Solef

    21216 + 1% whiskers

    Solef 21216

    composite Solef

    21216 + 6% whiskers

    composite Solef

    21216 + 9% whiskers

    composite Solef

    21216 + 12%

    whiskers

    X 3

    X 10

  • Main technical activities Electrolyte/Separator

    The electrolyte formulation based on new fluorinated solvents, salts based on sulfonimide, varying from fully or partially fluorinated, alkyl or alkoxy.

    At a first step solvents were tested with LiTFSI as a simple Sulfonimide.

    We work on the corrosion issue of the Alu collector linked to these electrolytes types at high voltage.

    The interactions between the different polymers and these electrolyte components have been analysed. Better understanding of the interaction with special PVDF copolymers and fluorinated solvents has been generated.

    Membranes

    Polymer/ Electrolyte interactions : Wettability at filling, homogeneity, safety of gel and effect on power.

    Electrolyte :

    Salt / Solvents /

    additives

    FluorinatedSalts

    Fluorinated Polymers

    FluorinatedSolvents

  • Main technical activities on half and full cells

    Full cells have been tested, with new cathode, new anode, and additives

    New dense and porous separators have been tested but thickness need to be reduced to decrease impedance and cost.

    First estimations has showed that with preliminary results the target of 200 Wh/kg would be achievable considering a cell voltage of 4,9V.

    0 5 10 15 20 250

    100

    200

    300

    400

    500

    Ch

    arg

    e c

    ap

    ab

    ilty

    C/102C1CC/2C/3C/5

    Amelie_SLALNMO_X23 T = 30C

    LNMO: 5.00 mg

    SLA-1025: 1.62 mg

    SLA-1025/LNMO: 0.82

    Electrolyte: LF30 + 1.6% F1EC + 2% SA

    Sp

    ecific

    ca

    pa

    city /

    mA

    h g

    -1

    SL

    A-1

    02

    5

    Cycle number

    Charge Discharge

    Discharge capability at 30 C

  • Life cycle analysis, end of life and recyclability

    Recycling

    Recycling at end of life aim to reach an overall target of 64%(gravimetric).

    All the newly designed AMELIE battery components of the batteries and the production routes are under evaluation in term of environmental impact.

    With a strong focus on the recycle rate target of EU Battery Directive EC/66/06 at the lowest possible cost.

    Eco-design.

    Eco-design follows the whole project process with recommendations for recycling/recovery/reuse.

    All routes using chemical way for recycling will be analysed against the requirements for REACH and ROHS.

    Besides the focus on electro active materials, the project will follow eco-design recommendations for electrolyte and membranes.

    The Eco-design will not be restricted to the recovery of inorganic materials (e.g. electrodes materials and current collectors), but a special attention will be paid to environmental friendly elaboration process, (including water based processes and extrusion of membranes)

  • Conclusion (Partial, for today..)

    Main achievement obtained on coin cells at Lab level. High voltage active materials giving access to 200 Wh/kg.

    Electrolyte improvement based on additives.

    First Separators at Lab level.

    Next steps. Scale up and optimize formulation.

    New selected salts and solvents for electrolyte under testing.

    Improve reliability of production of Separator at low thickness and the functionalization of the separator

    Major activities and deliverables in the coming year? Pilot cells to be cycled according to the projects specifications.

    Performances of electrolyte/separator set.

    What are the risks and challenges? Performances of electrolyte/separator set.

    Regarding cyclability

    Regarding Electrolyte (Al collector corrosion) and best fit with separator.

    Safety remains a question that cannot be solved on lab cells

    Extension of Topics that may need further collaborations. Characterising ageing and the contribution of the separator/electrolyte set to l