CN113793987A - High-performance intrinsic non-combustible lithium battery electrolyte taking lithium nitrate as lithium salt - Google Patents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0568—Liquid materials characterised by the solutes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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- H01M10/0567—Liquid materials characterised by the additives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0569—Liquid materials characterised by the solvents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
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- H01M2300/0091—Composites in the form of mixtures
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a high-performance intrinsic non-combustible lithium battery electrolyte taking lithium nitrate as lithium salt, which takes the lithium nitrate as main lithium salt or only lithium salt and comprises an organic solvent, an organic film-forming additive and the lithium salt; in the lithium battery electrolyte, the molar concentration of lithium salt is 0.5-2.8 mol/L. The lithium nitrate which is easy to be a conventional organic lithium salt is used as an ion conducting lithium salt, and a small amount of organic film forming additive is added, so that a novel electrolyte formula which is intrinsic and non-combustible, can efficiently inhibit lithium dendrite, is low in cost and simple in production process is compounded, the defects that the conventional secondary lithium battery is flammable and explosive in a high-temperature environment can be overcome, and the growth of dendritic lithium dendrite can be effectively inhibited.
Description
Technical Field
The invention belongs to the field of electrolyte of new energy batteries, and particularly relates to high-performance intrinsic non-combustible lithium battery electrolyte taking lithium nitrate as lithium salt.
Background
The emission of carbon dioxide gas generated during the combustion of carbon-containing combustible materials is reduced as soon as possible, and the development of clean and efficient new energy are imperative. Among the numerous clean new energy types, lithium batteries have developed particularly rapidly in recent decades by virtue of their many advantages, such as high energy density, long service life, wide application range, and the like. However, with the great increase of the energy density of the lithium battery, the safety problem becomes a key problem restricting the further development of the lithium battery.
On one hand, the safety problem of the lithium battery is caused by the fact that the electrolyte with low flash point and easy combustion is easy to generate thermal runaway and even explode under the conditions of thermal abuse, electrical abuse, mechanical abuse and the like; on the other hand, the growth of lithium dendrites during the cycle easily pierces the separator to cause internal short circuit, thereby inducing the occurrence of fire accidents. Therefore, the development of a high-performance and high-safety electrolyte having flame-retardant and even intrinsically non-combustible properties and simultaneously having a lithium dendrite-inhibiting effect is urgently needed.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-performance intrinsic non-combustible lithium battery electrolyte taking lithium nitrate as a lithium salt, which not only can solve the defects of flammability and explosiveness in a high-temperature environment of the conventional secondary lithium battery, but also can effectively inhibit the growth of dendritic lithium dendrites.
The intrinsic non-combustible lithium battery electrolyte is lithium nitrate as a main lithium salt or only lithium salt, and consists of an organic solvent, an organic film-forming additive (cosolvent), an inorganic film-forming additive and lithium salt.
The organic solvent is one or a mixture of more of trimethyl phosphate (TMP), triethyl phosphate (TEP), dimethyl methyl phosphonate (DMMP) and diethyl methyl phosphonate (DEMP).
The organic film forming additive (cosolvent) is one or more of fluoroethylene carbonate (FEC), Vinylene Carbonate (VC), Ethylene Sulfite (ES) and Propylene Sulfite (PS).
The inorganic film-forming additive is trifluoro-cyclic imide Lithium (LTFSI) or bis-trifluoromethylLithium alkylcycloimide (LITFSI) and lithium hexafluorophosphate (LIPF)6) One or more of lithium bis (oxalato) borate (LIBOB), lithium difluoro (oxalato) borate (LIDFOB).
The lithium salt is high-purity lithium nitrate (LINO)3)。
In the intrinsic non-combustible lithium battery electrolyte, the volume ratio of an organic solvent to an organic film forming additive (cosolvent) is 10: 0-5: 5, and the intrinsic non-combustible lithium battery electrolyte is different according to different organic film forming additive components on the premise that the electrolyte is non-combustible or flame retardant.
In the intrinsic non-combustible lithium battery electrolyte, the molar concentration of lithium salt is 0.5-2.8 mol/L, and the adjustment is specifically carried out according to the solvent property and the required performance.
In the intrinsic non-combustible lithium battery electrolyte, the molar concentration of the inorganic film-forming additive is 0-1.0 mol/L, the addition amount is usually low and is far lower than the concentration of lithium salt, and lithium nitrate is ensured to be used as the only lithium salt or main lithium salt.
The invention has the beneficial effects that:
different from the conventional combustible carbonate or organic ether electrolyte, the invention provides an intrinsic non-combustible electrolyte formula which takes organic phosphate as a unique solvent or a cosolvent, and simultaneously adopts inorganic lithium nitrate with high thermal stability and high water oxygen stability different from the conventional organic lithium salt as a main lithium salt or a unique lithium salt to obtain an SEI film with high ionic conductivity and rich inorganic phase; fluoroethylene carbonate (FEC), Vinylene Carbonate (VC), Ethylene Sulfite (ES) and Propylene Sulfite (PS) are used as organic film forming additives to improve the mechanical stability of the negative electrode SEI film. The non-combustible electrolyte with different properties is prepared by adjusting the proportion of the solvent and the additive, so that the problem that the conventional electrolyte is easy to burn is solved. Meanwhile, lithium nitrate is used as lithium salt and acts with the organic film forming additive together to generate the excellent effect of inhibiting lithium dendrite, so that the application of the lithium nitrate in the lithium metal battery becomes possible. Meanwhile, the high-stability lithium salt can greatly reduce the low-water and low-oxygen environment requirement of electrolyte preparation, is favorable for reducing the production cost and improving the production efficiency. It is worth mentioning that the electrolyte with lithium nitrate as the main lithium salt or the only lithium salt has a high electrochemical window (high voltage resistance), and the electrolyte shows extremely high capacity and cycle stability in the battery cycles of the high-nickel ternary NCM622, NCM811 and NCM90505, and has an excellent effect of stabilizing the high-nickel ternary positive electrode.
Drawings
FIG. 1 is a graph showing a comparison of the combustion performance of glass fiber membranes impregnated with different electrolytes, (a) commercial electrolytes; (b) TF91-2.2M non-combustible electrolyte. Compared with the commercial electrolyte which is extremely inflammable, the TF91-2.2M electrolyte has the characteristic of non-inflammability.
FIG. 2 is a graph showing the impedance comparison of electrolytes of different formulations. It can be seen from the graph that as the concentration of lithium nitrate increases, the impedance of the electrolyte shows a tendency of first decreasing rapidly and then increasing slowly; under the premise of unchanged concentration of lithium nitrate, the influence of the FEC content change on the impedance is small.
FIG. 3 is a comparison of electrochemical windows for different ratios of electrolyte formulations. The decomposition voltage of the electrolytes with different proportions is larger than 4.5V.
Fig. 4 is a graph comparing coulombic efficiencies in Li-Cu tests using electrolytes of different ratios. The graph shows that the electrolyte system has higher coulombic efficiency, which indicates that the electrolyte system has excellent lithium dendrite inhibiting property, and the circulating coulombic efficiency and stability can be further improved along with the increase of the concentration of the lithium nitrate.
FIG. 5 shows the cycle performance of two electrolytes, TEP-2.2M and TF91-2.2M, in a ternary NCM811 system. As can be seen from the figure, the electrolyte shows higher discharge capacity and coulombic efficiency in a ternary NCM811 system, and can obviously improve the cycling stability of the ternary NCM811 positive electrode.
FIG. 6 is a graph comparing the cycling performance of a commercial electrolyte and a TF91-2.2M electrolyte in a graphite anode system. As can be seen, the TF91-2.2M electrolyte has better cycling stability for the graphite negative electrode than the commercial electrolyte.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1:
1. raw material treatment: the 4A molecular sieve calcined at high temperature is used for carrying out dehydration treatment on solvent TMP and additive FEC, and high-purity lithium nitrate (99.99%) does not need to be treated;
2. dissolution of lithium salt: accurately sucking 18ml of TMP solution into a transparent sample bottle by using a pipette, accurately weighing 3.0338g of lithium nitrate, adding the lithium nitrate into the solution, accelerating dissolution by using stirring equipment, and properly heating by using a heating device until the lithium nitrate is completely dissolved;
3. adding an additive: accurately measuring 2ml of FEC by using a pipette, adding into the solution, shaking to uniformly mix the FEC and standing for later use;
4. assembling the lithium metal battery: the negative electrode is made of metal lithium; the anode is made of ternary nickel-cobalt-manganese NCM811 with the surface density of active substance of about 2.5mg/cm2(ii) a Assembling a button type lithium metal full battery by adopting a conventional lamination mode, and carrying out related tests;
5. assembling the lithium ion battery: the negative electrode is made of artificial graphite, and the surface density of the active substance is about 2.0mg/cm2(ii) a The conventional lamination mode is adopted to assemble a button type lithium ion half cell which takes metal lithium as a reference electrode, and then a cell circulating system is used for researching the compatibility of electrolyte and graphite.
Remarking: the above electrolyte preparation and cell assembly processes were performed in a glove box filled with argon.
Example 2:
1. raw material treatment: the solvent TEP and the additive FEC are subjected to dehydration treatment by using the 4A molecular sieve calcined at high temperature, and high-purity lithium nitrate (99.99%) does not need any treatment;
2. dissolution of lithium salt: accurately sucking 18ml of TEP solution into a transparent sample bottle by using a liquid-transferring gun, accurately weighing 3.0338g of lithium nitrate, adding the lithium nitrate into the solution, accelerating dissolution by using stirring equipment, and heating by using a heating device properly until the lithium nitrate is completely dissolved;
3. adding an additive: accurately measuring 2ml of FEC by using a pipette, adding into the solution, shaking to uniformly mix the FEC and standing for later use;
4. assembling the lithium metal battery: the negative electrode is made of metal lithium; the anode is made of ternary nickel-cobalt-manganese NCM811 with the surface density of active substance of about 2.5mg/cm2(ii) a Assembling a button type lithium metal full battery by adopting a conventional lamination mode, and carrying out related tests;
5. assembling the lithium ion battery: the negative electrode is made of artificial graphite, and the surface density of the active substance is about 2.0mg/cm2(ii) a The conventional lamination mode is adopted to assemble a button type lithium ion half cell which takes metal lithium as a reference electrode, and then a cell circulating system is used for researching the compatibility of electrolyte and graphite.
Remarking: the above electrolyte preparation and cell assembly processes were performed in a glove box filled with argon.
Example 3:
1. raw material treatment: the 4A molecular sieve after high-temperature calcination is used for carrying out dehydration treatment on the solvent TEP and the additive VC, and high-purity lithium nitrate (99.99%) does not need to be treated;
2. dissolution of lithium salt: accurately sucking 18ml of TEP solution into a transparent sample bottle by using a liquid-transferring gun, accurately weighing 3.0338g of lithium nitrate, adding the lithium nitrate into the solution, accelerating dissolution by using stirring equipment, and heating by using a heating device properly until the lithium nitrate is completely dissolved;
3. adding an additive: accurately measuring 2ml of VC by using a pipette, adding the VC into the solution, shaking to uniformly mix the VC and the solution, and standing for later use;
4. assembling the lithium metal battery: the negative electrode is made of metal lithium; the anode is made of ternary nickel-cobalt-manganese NCM811 with the surface density of active substance of about 2.5mg/cm2(ii) a Assembling a button type lithium metal full battery by adopting a conventional lamination mode, and carrying out related tests;
5. assembling the lithium ion battery: the negative electrode is made of artificial graphite, and the surface density of the active substance is about 2.0mg/cm2(ii) a The conventional lamination mode is adopted to assemble a button type lithium ion half cell which takes metal lithium as a reference electrode, and then a cell circulating system is used for researching the compatibility of electrolyte and graphite.
Remarking: the above electrolyte preparation and cell assembly processes were performed in a glove box filled with argon.
Example 4:
1. raw material treatment: the solvent TEP and the additive FEC are subjected to dehydration treatment by using the 4A molecular sieve calcined at high temperature, and high-purity lithium nitrate (99.99%) does not need any treatment;
2. dissolution of lithium salt: accurately sucking 18ml of TEP solution into a transparent sample bottle by using a liquid-transferring gun, accurately weighing 3.0338g of lithium nitrate, adding the lithium nitrate into the solution, accelerating dissolution by using stirring equipment, and heating by using a heating device properly until the lithium nitrate is completely dissolved;
3. adding an additive: accurately measuring 2ml of FEC by using a pipette, adding the FEC into the solution, shaking to uniformly mix the FEC, then adding 0.575g of organic lithium salt LiDFOB (0.2M) into the solution, stirring to completely dissolve the organic lithium salt, and standing for later use;
4. assembling the lithium metal battery: the negative electrode is made of metal lithium; the anode is made of ternary nickel-cobalt-manganese NCM811 with the surface density of active substance of about 2.5mg/cm2(ii) a Assembling a button type lithium metal full battery by adopting a conventional lamination mode, and carrying out related tests;
5. assembling the lithium ion battery: the negative electrode is made of artificial graphite, and the surface density of the active substance is about 2.0mg/cm2(ii) a The conventional lamination mode is adopted to assemble a button type lithium ion half cell which takes metal lithium as a reference electrode, and then a cell circulating system is used for researching the compatibility of electrolyte and graphite.
Remarking: the above electrolyte preparation and cell assembly processes were performed in a glove box filled with argon.
Example 5:
1. raw material treatment: the solvent TEP and the additive FEC are subjected to dehydration treatment by using the 4A molecular sieve calcined at high temperature, and high-purity lithium nitrate (99.99%) does not need any treatment;
2. dissolution of lithium salt: accurately sucking 18ml of TEP solution into a transparent sample bottle by using a liquid-transferring gun, accurately weighing 2.0685g of lithium nitrate, adding the lithium nitrate into the solution, accelerating dissolution by using stirring equipment, and heating by using a heating device properly until the lithium nitrate is completely dissolved;
3. adding an additive: accurately measuring 2ml of FEC by using a pipette, adding into the solution, shaking to uniformly mix the FEC and standing for later use;
4. assembling the lithium metal battery: the negative electrode is made of metal lithium; the anode is made of ternary nickel-cobalt-manganese NCM811 with the surface density of active substance of about 2.5mg/cm2(ii) a Assembling a button type lithium metal full battery by adopting a conventional lamination mode, and carrying out related tests;
5. assembling the lithium ion battery: the negative electrode is made of artificial graphite, and the surface density of the active substance is about 2.0mg/cm2(ii) a The conventional lamination mode is adopted to assemble a button type lithium ion half cell which takes metal lithium as a reference electrode, and then a cell circulating system is used for researching the compatibility of electrolyte and graphite.
Remarking: the above electrolyte preparation and cell assembly processes were performed in a glove box filled with argon.
Example 6:
1. raw material treatment: the solvent TEP and the additive FEC are subjected to dehydration treatment by using the 4A molecular sieve calcined at high temperature, and high-purity lithium nitrate (99.99%) does not need any treatment;
2. dissolution of lithium salt: accurately sucking 15ml of TEP solution into a transparent sample bottle by using a liquid-transferring gun, accurately weighing 2.0685g of lithium nitrate, adding the lithium nitrate into the solution, accelerating dissolution by using stirring equipment, and heating by using a heating device properly until the lithium nitrate is completely dissolved;
3. adding an additive: accurately measuring 5ml of FEC by using a pipette, adding the FEC into the solution, shaking to uniformly mix the FEC and standing for later use;
4. assembling the lithium metal battery: the negative electrode is made of metal lithium; the anode is made of ternary nickel-cobalt-manganese NCM811 with the surface density of active substance of about 2.5mg/cm2(ii) a Assembling a button type lithium metal full battery by adopting a conventional lamination mode, and carrying out related tests;
5. assembling the lithium ion battery: the negative electrode is made of artificial graphite, and the surface density of the active substance is about 2.0mg/cm2(ii) a Button-type lithium ion half parts respectively assembled by conventional lamination mode and using metal lithium as reference electrodeThe compatibility of the electrolyte and graphite was investigated with the battery followed by a battery circulation system.
Remarking: the above electrolyte preparation and cell assembly processes were performed in a glove box filled with argon.
Claims (6)
1. A high-performance intrinsic non-combustible lithium battery electrolyte taking lithium nitrate as lithium salt is characterized in that:
the lithium battery electrolyte is lithium nitrate serving as a main lithium salt or a unique lithium salt and comprises an organic solvent, an organic film-forming additive and a lithium salt; in the lithium battery electrolyte, the molar concentration of lithium salt is 0.5-2.8 mol/L.
2. A lithium battery electrolyte as claimed in claim 1, characterized in that:
the organic film forming additive is one or more of fluoroethylene carbonate, vinylene carbonate, ethylene sulfite and propylene sulfite.
3. A lithium battery electrolyte as claimed in claim 1, characterized in that:
the organic solvent is one or a mixture of trimethyl phosphate, triethyl phosphate, dimethyl methyl phosphonate and diethyl methyl phosphonate.
4. A lithium battery electrolyte as claimed in claim 1, 2 or 3, characterized in that:
the volume ratio of the organic solvent to the organic film-forming additive is 10: 0-5: 5.
5. A lithium battery electrolyte as claimed in claim 1, characterized in that:
the lithium battery electrolyte also comprises an inorganic film-forming additive; the inorganic film-forming additive is one or more of trifluoro-cyclic imide lithium, bis-trifluoro-methane cyclic imide lithium, lithium hexafluorophosphate, lithium dioxalate borate and lithium difluorooxalate borate.
6. A lithium battery electrolyte as claimed in claim 5, characterized in that:
in the lithium battery electrolyte, the molar concentration of the inorganic film-forming additive is 0-1.0 mol/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114400380A (en) * | 2022-01-21 | 2022-04-26 | 中国科学技术大学 | Multi-effect lithium battery electrolyte with functions of inhibiting growth of lithium dendrite, optimizing electrochemical performance and efficiently retarding flame |
| WO2023201393A1 (en) * | 2022-04-21 | 2023-10-26 | The University Of Adelaide | Improved electrolyte for batteries |
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| US20020151631A1 (en) * | 2001-01-31 | 2002-10-17 | Ishizuka Garasu Kabushiki Kaisha | Flame-retardant material and flame-retardant polymer material |
| WO2002095100A1 (en) * | 2001-05-24 | 2002-11-28 | Toray Industries, Inc. | Flame-resistant fiber material, carbon fiber material, graphite fiber material and method for production thereof |
| CN105264692A (en) * | 2013-06-07 | 2016-01-20 | 大众汽车有限公司 | New electrolyte composition for high-energy anodes |
| CN110048163A (en) * | 2019-04-10 | 2019-07-23 | 中国科学院化学研究所 | A kind of lithium metal battery flame-retardant electrolyte and its preparation method and application |
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2021
- 2021-09-17 CN CN202111091185.8A patent/CN113793987A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20020151631A1 (en) * | 2001-01-31 | 2002-10-17 | Ishizuka Garasu Kabushiki Kaisha | Flame-retardant material and flame-retardant polymer material |
| WO2002095100A1 (en) * | 2001-05-24 | 2002-11-28 | Toray Industries, Inc. | Flame-resistant fiber material, carbon fiber material, graphite fiber material and method for production thereof |
| CN105264692A (en) * | 2013-06-07 | 2016-01-20 | 大众汽车有限公司 | New electrolyte composition for high-energy anodes |
| CN110048163A (en) * | 2019-04-10 | 2019-07-23 | 中国科学院化学研究所 | A kind of lithium metal battery flame-retardant electrolyte and its preparation method and application |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114400380A (en) * | 2022-01-21 | 2022-04-26 | 中国科学技术大学 | Multi-effect lithium battery electrolyte with functions of inhibiting growth of lithium dendrite, optimizing electrochemical performance and efficiently retarding flame |
| WO2023201393A1 (en) * | 2022-04-21 | 2023-10-26 | The University Of Adelaide | Improved electrolyte for batteries |
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