• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a method for forming a Li-ion battery cell comprising a positive electrode material having a porosity ranging from 20 to 35% and comprising at least one sacrificial salt, a negative electrode material, a separator and an electrolyte, comprising the following successive steps: (a) heating the cell to a temperature Ti ranging from 30 to 45 ° C; (b) charging the cell to a potential of less than or equal to 4.8 V, preferably ranging from 4.6 to 4.8 V, more preferably from 4.7 to 4.8 V.
    公开号:FR3040547A1
    申请号:FR1558138
    申请日:2015-09-02
    公开日:2017-03-03
    发明作者:Bruno Delobel；Mohamed Chakir；Yvan Reynier；Florence Masse
    申请人:Renault SAS；
    IPC主号:
    专利说明:

    The invention relates to the general field of rechargeable lithium-ion batteries. The invention more specifically relates to a method of forming a battery cell comprising a positive electrode material comprising at least one sacrificial salt.
    Conventionally, the Li-ion batteries comprise one or more cathodes, one or more anodes, an electrolyte and a separator composed of a porous polymer or any other suitable material in order to avoid any direct contact between the electrodes.
    Li-ion batteries are already widely used in many mobile applications. This trend can be explained in particular by densities of mass and volume energy that are much higher than those of conventional nickel cadmium (Ni-Cd) and nickel-metal hydride (Ni-MH) batteries, a lack of memory effect, and a low self-discharge. compared to other accumulators and also by a drop in costs per kilowatt-hour related to this technology. Nevertheless, an improvement of this technology is needed to win new markets such as electric and hybrid vehicles that often require high energy density, high power density and long life.
    Once the Li-ion battery cell is activated, ie when the assembly of the cell is made and the electrolyte is impregnated in the cell, thermodynamic reactions are initiated during the first charge cycle of the cell. said cell and the first lithium ion exchanges between the electrodes take place. Products resulting from these reactions accumulate on the surface of the electrodes to form a layer called "Solid Electrolyte"
    Interphase "(SEI). This layer is an essential element for the proper functioning of the Li-ion battery, because not only does it conduct lithium ions very well, but it also has the advantage of stopping the catalytic decomposition of the solvent. Nevertheless, it is known that the batteries lose between 5 and 20% of the potential capacity of their positive electrode, thus limiting the energy density of said batteries, during the formation of this layer during which the negative electrode consumes energy. irreversibly.
    In order to solve this problem, several approaches have been considered.
    Thus, metallic lithium has been added to the negative electrode to compensate for irreversible lithium consumption during the first charge cycle as described in JP 2012/009209. However, the implementation of lithium metal state poses many problems because it reacts violently with moisture and polar solvents commonly used in the implementation of electrode inks (usually water or N- methylpyrrolidone (NMP)).
    A sacrificial salt may also be added to the positive electrode as described in document FR 2 961 634. A particular lithium oxalate salt is disclosed in this patent, but is considered unsuitable because it oxidizes at too high a potential.
    Furthermore, additives have been introduced into the electrolyte, such as vinylene carbonate as well as Aurbach et al. In "On the use of vinylene carbonate (VC) as an additive to electrolyte solutions for Li-ion batteries" Electrochemica Acta 47 (2002), 1423-1439, or else propane carbonate as Zuo et al contemplates in "Electrochemical reduction of 1,3-propane sultone on graphite electrodes and its application in Li-ion batteries" Electrochemica and Solid-State Letters 9 (4), A196-A199 (2006), to improve the quality of the SEI thus playing a role in the life of the cell.
    However, the major disadvantage related to the use of additives is associated with the lithium consumption of the positive electrode for the formation of the SEI layer. This has an impact on the initial capacity of the cell but also on the total life cycle of said cell.
    The present invention aims to propose a solution to solve the problem related to the irreversible capacity due to the first training cycle of Li-ion batteries and to increase the durability of said batteries.
    According to the invention, a method of forming a Li-ion battery cell comprising a positive electrode material having a porosity ranging from 20 to 35% and comprising at least one sacrificial salt, a negative electrode material, a separator and an electrolyte, comprises the following successive steps: (a) heating the cell to a temperature Ti ranging from 30 to 45 ° C; (b) charging the cell to a potential of less than or equal to 4.8 V, preferably ranging from 4.6 to 4.8 V, more preferably from 4.7 to 4.8 V.
    The method according to the invention makes it possible to significantly reduce the loss of capacitance of the positive electrode of the Li-ion battery cell during the first charge cycle, thereby increasing the lifetime of said battery. Other advantages and characteristics of the invention will appear more clearly on examination of the detailed description and the attached drawings in which: FIG. 1 is a graph showing the evolution of the potential of three Li-ion battery cells in function of time; FIG. 2 is a graph showing the evolution of the discharge capacity and the evolution of the internal resistance of three Li-ion battery cells, as a function of the number of cycles; FIG. 3 is a graph showing the evolution of the discharge capacity and the evolution of the resistance of three Li-ion battery cells exhibiting particular porosity levels, as a function of the number of cycles.
    In the description of the invention, the term "based on" is synonymous with "comprising predominantly".
    It is furthermore specified that the expressions "from ... to ..." used in the present description must be understood as including each of the mentioned terminals.
    As explained above, the forming method according to the invention relates to a Li-ion battery cell comprising a positive electrode material having a porosity level ranging from 20 to 35% and comprising at least one sacrificial salt, a negative electrode material. , a separator and an electrolyte.
    The actual density of the electrode (Dr) is calculated from the mass and the thickness of the electrode deposit. Thanks to the densities of each component, the theoretical density (compact) of deposit (Dth) can be calculated. Thus, the porosity level (tP, expressed as a percentage), defined as the void ratio within the electrode, is given by the following equation (I): tP = (1 - Dr / Dth) * 100 ( I).
    The sacrificial salt is a compound capable of oxidizing during the first charging cycle of the assembled battery cell, to a potential ranging for example from 2 to 5 V. During its oxidation, the sacrificial salt produces ions (ions Li + when the sacrificial salt is a salt of the cation Li +) which enter the electrolyte. It is said that said salt has pre-lithic properties. Said ions at least partially compensate for the capacity lost during the formation of the SEI layer on the negative electrode.
    In addition, the oxidized salt creates a porosity within the electrode which must be finely controlled in order to avoid a loss of performance of the Li-ion accumulator. Indeed too high porosity limits the electronic contacts between particles and increases the resistance of the electrochemical cell.
    According to one particular embodiment of the invention, the sacrificial salt is chosen from L12C204, L1N3, L12C305, L12C4O6, L12C3O3, L12C4O4, L12C5O5, L12C6O6, L12N4O2 and [L12N2C2O2] η, π ranging from 1 to 100, preferably from 1 to 50, more preferably 1 to 10, preferably L12C2O4. Lithium oxalate is a salt with a capacity of 545 mAh / g, stable in air, which can be integrated in a positive electrode formulation. Between 4.5 and 5.5V vs. Li + / Li, it oxidizes by releasing carbon dioxide and two lithium ions. The released lithium ions make it possible to compensate for the irreversible capacity of first charge of a Li-ion battery cell, thus increasing its initial capacity. Carbon dioxide is removed at the end of training, and its mass (function of the oxalate level) does not contribute to that of the battery.
    According to another characteristic of the invention, the material for a positive electrode comprises from 3 to 10% by weight of sacrificial salt, preferably from 3 to 7%, more preferably from 4 to 6%, relative to the total weight of the positive electrode.
    Advantageously, the porosity of the positive electrode is 25 to 35%.
    Preferably, the material for positive electrode comprises an active material chosen from: phosphates of olivine structure LivTaP04, in which
    and Ta is selected from Fe, Ni, Co, Mn and mixtures thereof; the materials of formula Li 1 + u (MaDb) i-uO 2, in which
    , M is selected from Ni, Mn, Co and mixtures thereof, D represents a metal or a plurality of doping metals selected from Na, Zn, Cd, Mg, Ti, Ca, Zr, Sr, Ba, Al and K
    and a + b = 1; and spinel structure materials selected from LiMn 2 O 4 and LiNi 3 Mn 5 O 4, more preferentially olivine structure phosphates, still more preferably LiFePCL.
    The oxidation potential of lithium oxalate is too high to be used with a number of positive electrodes, such as the LiNixMnyCoz02 (NMC) based electrode, where x + y + z = 1, the electrode based on LiNiO.8Coo.15Alo.05O2 (NCA) or the L1COO2 (LCO) based electrode whose structure is unstable above 4.5V.
    However, with spinel type materials (LiMn204 or LiNiO.5Mn1.5O4) or lithium phosphate Li (Fe, Mn, Ni) PO4, or of the type (Lii + XM02), potentials of 5V can be envisaged, because either the field of activity of these materials is confounded with the activation potential of oxalate, or it is totally disjoint. For example with a material of LiFePO4 type, the redox activity is between 3.4V and 3.5V, and does not oxidize further. By adding the oxalate salt, it can be oxidized at 5V without the risk of disturbing the structure of the active material.
    However, it is known that the standard electrolytes of Li-ion (carbonate-based) batteries begin to oxidize above 4V, a phenomenon that becomes predominant beyond 5V. It is therefore desirable to minimize the maximum charge potential to avoid these parasitic reactions.
    Preferably, the positive electrode material comprises one or more binders.
    Preferably, the binder (s) are organic polymers, preferably polybutadiene-styrene latices, polyesters, polyethers, methylmethacrylate polymer derivatives, acrylonitrile polymer derivatives, carboxyl methyl cellulose, and derivatives thereof. polyvinyl acetates or polyacrylate acetate, polyvinylidene fluoride, and mixtures thereof.
    According to a variant of the method according to the invention, the material for negative electrode is based on graphite. The graphite carbon may be chosen from synthetic graphite carbons, and natural from natural precursors followed by purification and / or post-treatment. Other active carbon-based materials can be used such as pyrolytic carbon, amorphous carbon, activated carbon, coke, coal tar pitch and graphene. Mixtures of graphite with one or more of these materials are possible. Materials having a core-shell structure may be used when the core comprises high capacity graphite and when the shell comprises a carbon-based material protecting the core from degradation related to the repeated phenomenon of intercalation / deintercalation of lithium ions .
    Advantageously, the negative electrode material is based on a composite selected from a composite of silicon / graphite, tin / graphite, tin oxide / graphite, such as SnC 2 / graphite, and mixtures thereof, preferably a silicon / silicon composite. graphite.
    Preferably, the silicon / graphite composite comprises from 0 to 30% by weight of silicon relative to the total weight of the composite, more preferably from 0 to 15%, even more preferably from 5 to 10%.
    Preferably, the separator is located between the electrodes and acts as an electrical insulator. Several materials can be used as separators. The separators are generally composed of porous polymers, preferably polyethylene and / or polypropylene.
    Advantageously, the separator used is the Celgard® 2325 separator, that is to say a microporous single-layer membrane with a thickness of 25 μm composed of polypropylene.
    Preferably, said electrolyte is a liquid electrolyte.
    According to another characteristic of the invention, said electrolyte comprises one or more lithium salts.
    Advantageously, said one or more lithium salts are chosen from lithium bis [(trifluoromethyl) sulphonyl] imide (LiN (CF 3 80 2) 2), lithium trifluoromethane sulphonate (L1CF3SO3), lithium bis (oxalato) borate (LiBOB), lithium bis (perfluoroethylsulphonyl) imide (LiN (CF3CF2SO2) 2), L1CIO4, LiAsF6, LiPF6, LiBF4, L1, L1CH3SO3, LiB (C204) 2, LiRFSOSRF, LiN (RFSO2) 2, LiC (RFSO2) 3, Rf being a grouping selected from a fluorine atom and a perfluoroalkyl group having from one to eight carbon atoms.
    Preferably, the electrolyte comprises a solvent mixture comprising ethylene carbonate and at least one solvent selected from ethyl and methyl carbonate, dimethyl carbonate, diethyl carbonate and mixtures thereof.
    According to one particular embodiment of the invention, the electrolyte comprises a mixture of ethylene carbonate, dimethyl carbonate and ethyl and methyl carbonate at a ratio 1/1/1 by volume with the sodium salt. lithium LiPF6 to IM.
    As mentioned above, step (a) of the forming method according to the invention consists in heating the cell at a temperature Ti ranging from 30 to 45 ° C.
    Preferably, the temperature T 1 is from 35 to 45 ° C, more preferably the temperature T 1 is 40 ° C.
    As explained above, step (b) of the forming method according to the invention consists of a charge of the cell up to a potential of less than or equal to 4.8 V, preferably ranging from 4.6 to 4. , 8 V, more preferably 4.7 to 4.8 V. More preferably, the charge of the cell is carried out up to a potential ranging from 4.75 to 4.8V.
    According to a particular embodiment of the invention, a forming method according to the invention, applied to a battery cell comprising a material for positive electrode having a porosity level ranging from 20 to 35%, preferably 35%, said material comprising an active material of formula LiFePO 4 and 5% by weight of lithium oxalate with respect to the total weight of the positive electrode, a negative electrode material, a separator and an electrolyte, comprises the following successive steps: ) heating the cell at a temperature Ti of 40 ° C; (b) a charge of the cell up to a potential of 4.7 to 4.8 V, preferably 4.8 V.
    EXAMPLES 1. Preparation of a Li-ion battery cell comprising a positive electrode comprising lithium oxalate 1.1 Preparation of a positive electrode
    An active material of formula LiFePCU is used. The positive electrode is prepared by mixing 85% by weight of active material, 5% by weight of a Super P® carbon additive, 5% by weight of polyvinylidene fluoride in N-methyl-2-pyrrolidone (NMP) and 5% by weight lithium oxalate Li2C204. The electrode is made by depositing the mixture on a 20 μm thick aluminum foil. The electrode is dried and calendered at 80 ° C. 1.2 Preparation of a negative electrode
    A negative electrode based on a silicon / graphite composite (Hitachi Chemical) was prepared. The negative electrode is prepared by mixing 94% by weight of active material, 2% by weight of carboxymethylcellulose (CMC), and 4% by weight of Styrofan® latex, that is to say a carboxylated styrene-butadiene copolymer. The electrode is made by depositing the mixture on a 10 μm thick copper foil. The electrode is dried and calendered at 80 ° C. 1.3 Separator
    The Celgard® 2325 separator is used to prevent short-circuiting between the positive electrode and the negative electrode during charge and discharge cycles. The Celgard® 2325 separator is a 25 μm monolayer microporous membrane made of polypropylene. 1.4 Electrolyte The electrolyte used is composed of 1M LiPF6 lithium salt dissolved in a mixture of ethylene carbonate, dimethyl carbonate and ethyl and methyl carbonate at a ratio 1/1/1 by volume. 1.5 Electrochemical cell
    A Li-ion battery cell is assembled by stacking the positive electrode, with a surface area of 10 cm 2, and the negative electrode as described above, the separator, as described above, being located between the electrodes, then the cell is impregnated with the electrolyte, as described above. 2. Electrochemical performance of the battery cell
    Li-ion 2.1 Evaluation of the variation of the potential of the Li-ion battery cell as a function of time Method
    Three particular forming processes, respectively named Method A, Method B, and Method C, were applied to the Li-ion battery cell as prepared above.
    Method A is applied to the Li-ion battery cell named cell A. Method B is applied to the cell named cell B and method C is applied to the cell named cell C.
    The comparative method A comprises a step of heating cell A to 22 ° C. and then a step of charging cell A to a potential of 4.8 V.
    Process B according to the invention comprises a step of heating cell B to 40 ° C and then a step of charging cell B to a potential of 4.8 V.
    Comparative process C comprises a step of heating cell C to 50 ° C. and then a step of charging cell C to a potential of 4.8 V. Result
    In FIG. 1, the curves A, B and C respectively correspond to the evolution of the potential of cells A, B and C.
    Figure 1 clearly shows that cells B and C exhibit electrochemical behavior different from that of cell A.
    When the potential is close to 3.2-3.3 V, the 3 curves have a plateau which corresponds to the redox activity of the active material of formula LiFePCL.
    When the potential is close to 4.8 V, curve A has a plateau which corresponds to the redox activity of lithium oxalate. On the other hand, curves B and C have a plateau, which also corresponds to the redox activity of lithium oxalate, when the potential is of the order of 4.5 V.
    Thus, FIG. 1 shows that an increase in the temperature of 22 to 40-50 ° C allows activation of the lithium oxalate at a lower potential so that it is possible to reduce the end-of-charge potential. at 4.8 V.
    This represents a very interesting advantage because the conventional electrolytes of Li-ion battery, that is to say based on carbonate solvents, are unstable at a potential greater than 5 V. 2.2 Evaluation of the variation the discharge capacity and the internal resistance of the Li-ion battery cell as a function of the number of cycles
    The method is identical to that mentioned in paragraph 2.1. Result
    In FIG. 2, the curve Al corresponds to the evolution of the discharge capacity of the cell A and the curve A2 corresponds to the evolution of the internal resistance of the cell A. The curve B1 corresponds to the evolution of the discharge capacity of the cell B and the curve B2 corresponds to the evolution of the internal resistance of the cell B. The curve C1 corresponds to the evolution of the discharge capacity of the cell C and the curve C2 corresponds to the evolution of the internal resistance of the C cell.
    FIG. 2 shows that a low discharge capacity is observed after 300 cycles (curve A1), and that the internal resistance of cell A increases significantly with the number of cycles (curve A2).
    On the other hand, good discharge capacities are observed for cells B and C according to curves B1 and C1. Cell C has a higher internal resistance (curve C2) than that of cell B (curve B2). Indeed, a too high temperature and the potential of 4.8 V lead to a high internal resistance due to the degradation of the electrolyte during the activation of the sacrificial salt, lithium oxalate.
    Thus, it is clearly shown that heating the cell at a temperature around 40 ° C, ranging from 30 to 45 ° C, is ideal to obtain both a low and stable internal resistance, a good discharge capacity and good cycling. 2.3 Evaluation of the variation of the discharge capacity and the internal resistance of Li-ion battery cells with particular porosity levels, as a function of the number of cycles
    The formation process B according to the invention was applied to three Li-ion battery cells, called cell D, cell E and cell F, each comprising a positive electrode, each of the positive electrodes having three different porosity levels, respectively of 47%, 35% and 42%, obtained by three different levels of calendering.
    Thus, a comparative forming method D was applied to cell D; a formation method E according to the invention has been applied to the cell E; a comparative F training method was applied to the F cell.
    In FIG. 3, the curve DI corresponds to the evolution of the discharge capacity of the cell D and the curve D2 corresponds to the evolution of the resistance of the cell D. The curve El corresponds to the evolution of the capacitance discharge of the cell E and the curve E2 corresponds to the evolution of the resistance of the cell E. The curve Fl corresponds to the evolution of the discharge capacity of the cell F and the curve F2 corresponds to the evolution of the resistance of cell F.
    FIG. 3 shows that cell D has a high internal resistance (curve D2), a low discharge capacity and poor cyclability (curve D1).
    The cell E has a low resistance (curve E2) and a good discharge capacity (curve El).
    The cell F has a relatively high internal resistance (curve F2) and a good discharge capacity (curve F1).
    Thus, it is shown that a porosity of 35% in the positive electrode makes it possible to obtain both a low and stable internal resistance, a good discharge capacity and a good cyclability.
    Beyond a porosity of 35%, the electrical conductivity of the positive electrode is limited and the resistance of the battery increases dramatically. In fact, the battery performance drops.
    权利要求:
    Claims (10)
    [1" id="c-fr-0001]
    A method of forming a Li-ion battery cell comprising a positive electrode material having a porosity ranging from 20 to 35% and comprising at least one sacrificial salt, a negative electrode material, a separator and an electrolyte , characterized in that it comprises the following successive steps: (a) heating the cell to a temperature Ti ranging from 30 to 45 ° C; (b) charging the cell to a potential of less than or equal to 4.8 V, preferably ranging from 4.6 to 4.8 V, more preferably from 4.7 to 4.8 V.
    [2" id="c-fr-0002]
    2. Method according to claim 1, wherein the sacrificial salt is chosen from L12C2O4, L1N3, L12C3O5, L12C4O6, L12C3O3, L12C4O4, L12C5O5, L12C6O6, L12N4O2 and [L12N2C2O2] η, π ranging from 1 to 100; preferably L12C2O4.
    [3" id="c-fr-0003]
    The method of claim 1 or 2, wherein the positive electrode material comprises from 3 to 10%, preferably from 3 to 7%, more preferably from 4 to 6%, by weight of sacrificial salt by weight. total of the positive electrode.
    [4" id="c-fr-0004]
    4. A method according to any one of the preceding claims, wherein the positive electrode material comprises an active material selected from: olivine structure phosphates LivTaP04, wherein

    and Ta is selected from Fe, Ni, Co, Mn and mixtures thereof; the materials of formula Li 1 + u (MaDb) i-uO 2, in which

    , M is selected from Ni, Mn, Co and mixtures thereof, D represents a metal or a plurality of doping metals selected from Na, Zn, Cd, Mg, Ti, Ca, Zr, Sr, Ba, Al and K

    and a + b = 1; and spinel structure materials selected from LiMn 2 O 4 and LiNi 3 Mn 2 O 4, more preferably the olivine structure phosphates, still more preferably LiFePO 4.
    [5" id="c-fr-0005]
    The method of any one of the preceding claims, wherein the positive electrode material comprises one or more binders.
    [6" id="c-fr-0006]
    The method of any of the preceding claims, wherein the negative electrode material is graphite-based.
    [7" id="c-fr-0007]
    The method of any of the preceding claims, wherein said electrolyte comprises one or more lithium salts.
    [8" id="c-fr-0008]
    8. Method according to the preceding claim, wherein said lithium salt (s) are chosen from lithium bis [(trifluoromethyl) sulphonyl] imide (LiN (CF3 8 () 2) 2), lithium trifluoromethanesulfonate (L1CF3SO3). ), lithium bis (oxalato) borate (LiBOB), lithium bis (perfluoroethylsulfonyl) imide (LiN (CF3CF2SO2) 2), L1CIO4, LiAsFg, LiPF6, LiBF4, Lil, L1CH3SO3, LiB (C204) 2, L1RfSOSRf, L1N ( RfSO2) 2, L1C (RfSO2) 3, Rf being a group selected from a fluorine atom and a perfluoroalkyl group having from one to eight carbon atoms.
    [9" id="c-fr-0009]
    9. Process according to any one of the preceding claims, in which the said electrolyte comprises a solvent mixture comprising ethylene carbonate and at least one solvent chosen from ethyl and methyl carbonate, dimethyl carbonate and carbonate. of diethyl and mixtures thereof.
    [10" id="c-fr-0010]
    10. Process according to any one of the preceding claims, wherein the temperature Ti is from 35 to 45 ° C, more preferably the temperature Ti is 40 ° C.
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    2017-03-03| PLSC| Publication of the preliminary search report|Effective date: 20170303 |
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    2021-06-11| ST| Notification of lapse|Effective date: 20210506 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1558138A|FR3040547B1|2015-09-02|2015-09-02|METHOD FOR FORMING A LI-ION BATTERY CELL EQUIPPED WITH A POSITIVE ELECTRODE COMPRISING A SACRIFICIAL SALT|FR1558138A| FR3040547B1|2015-09-02|2015-09-02|METHOD FOR FORMING A LI-ION BATTERY CELL EQUIPPED WITH A POSITIVE ELECTRODE COMPRISING A SACRIFICIAL SALT|
    KR1020187008559A| KR102084245B1|2015-09-02|2016-08-24|Method for forming a cell of a lithium-ion battery provided with a positive electrode comprising a sacrificial salt|
    CN201680054568.9A| CN108028357B|2015-09-02|2016-08-24|Method for forming a lithium-ion battery cell provided with a positive electrode comprising a sacrificial salt|
    EP16763923.6A| EP3345234B1|2015-09-02|2016-08-24|Method for forming a cell of a lithium-ion battery provided with a positive electrode comprising a sacrificial salt|
    PCT/FR2016/052111| WO2017037363A1|2015-09-02|2016-08-24|Method for forming a cell of a lithium-ion battery provided with a positive electrode comprising a sacrificial salt|
    JP2018511149A| JP6784753B2|2015-09-02|2016-08-24|A method for forming a cell of a lithium ion battery having a positive electrode containing a sacrificial salt|
    US15/756,625| US20180219250A1|2015-09-02|2016-08-24|Method for forming a cell of a lithium-ion battery provided with a positive electrode comprising a sacrificial salt|
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