CN110828894A - High-safety electrolyte and lithium ion battery thereof - Google Patents
High-safety electrolyte and lithium ion battery thereof Download PDFInfo
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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
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- H—ELECTRICITY
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- 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
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- 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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Abstract
The invention provides a high-safety electrolyte and a lithium ion battery thereof, wherein the high-safety electrolyte comprises a film-forming agent; the film forming agent is at least one of additive I or additive II. The electrolyte used by the lithium ion battery contains an inorganic film-forming agent and a long-chain organic film-forming agent, and a graphite-thin inorganic SEI film-loose thick organic SEI film is formed by controlling the molecular structure of the film-forming agent and matching with a proper pre-charging system, so that the electronic impedance of a negative electrode is increased, and the safety of the battery is improved.
Description
Technical Field
The invention belongs to the field of lithium ion batteries, and particularly relates to a high-safety electrolyte and a lithium ion battery thereof.
Background
With the improvement of the energy density of the lithium ion battery, the thickness of the diaphragm is thinner and thinner, and the probability of internal short circuit caused by burrs is greatly increased. Meanwhile, the diaphragm becomes thin, so that the thermal stability of the diaphragm becomes poor, and the thermal shrinkage of the diaphragm is increased when the battery is heated, so that the short circuit risk of the anode and the cathode is caused.
In the aspect of mechanical abuse, the lithium ion battery may encounter unexpected situations such as puncture and extrusion during use, and may cause serious internal short circuit.
The internal short circuit fire is caused by the fact that the aluminum foil is in contact with the negative electrode, and the aluminum foil and the negative electrode are very small in resistance, so that short circuit current is large, heat quantity is high, and the thermal runaway temperature of the reaction of the negative electrode and electrolyte is reached. The thought of improving the safety of short circuit, acupuncture and the like in the battery is probably three: one is to make a porous insulating coating on the surface of the diaphragm or the negative electrode; one is that a material with high insulating property is mixed in the negative electrode to reduce the overall conductivity of the negative electrode; the third is that a heat-sensitive coating is added on the diaphragm or the negative electrode, so that the diaphragm or the negative electrode has conductivity at low temperature and insulation at high temperature.
The coating type or the blending type materials increase the volume and the weight of the battery and reduce the energy density of the battery.
The conventional electrolyte additive is composed of an inorganic film-forming agent and an organic film-forming agent, and a thin SEI film is formed on the surface of a negative electrode during pre-charging. Most of the additives are small-molecule additives, and the formed film is also very thin. Since the SEI film has an insulating property, it is generally considered to reduce the thickness of the SEI film as much as possible to reduce battery resistance and improve power performance.
Disclosure of Invention
In view of the above, the present invention is directed to a high safety electrolyte and a lithium ion battery thereof, which have high molecular toughness and can reduce the cracking of the SEI film during the charge and discharge expansion of the negative electrode.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a high-safety electrolyte comprises an organic film-forming agent; the organic film forming agent is at least one of an agent I or an agent II;
the structural formula of the reagent I is as follows:
the structural formula of the reagent II is as follows:
further, n is1=1-5;n2=1-5。
Furthermore, the addition amount of the organic film forming agent is 0.5-5%.
Further, the electrolyte also comprises an electrolyte solvent, an electrolyte lithium salt and an inorganic film forming agent; the electrolyte solvent, the electrolyte lithium salt and the inorganic film-forming agent are as follows in parts by mass:
72-94 parts of an electrolyte solvent,
6-18 parts of lithium salt of the electrolyte,
0.5-5 parts of inorganic film forming agent.
Further, the electrolyte solvent is a combination of cyclic carbonate and chain carbonate; the cyclic carbonate is at least one of ethylene carbonate, propylene carbonate, butylene carbonate, alpha-butyrolactone or alpha-valerolactone; the chain carbonate is at least one of dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, diethoxyethane or 1, 3-dioxolane.
Further, the lithium salt of the electrolyte is LiPF6、LiBF4、LiClO4、LiBOB、LiN(CF3SO2)2Or Li (CF)3SO2)3At least one of; the concentration of the lithium salt of the electrolyte is 0.5-1.5M.
Further, the inorganic film forming agent is at least one of lithium difluorophosphate, vinylene carbonate or propylene sulfite.
A high-safety lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm and the electrolyte.
Further, the pre-charging temperature of the electrolyte is 10-100 ℃; the thickness of the pre-charged SEI film is more than or equal to 40 nm.
The positive electrode comprises a positive metal current collector, a positive active material, a conductive agent, a binder and a solvent; the positive metal current collector is an aluminum foil; the front partThe anode active material is lithium transition metal composite oxide, the mass of the anode active material accounts for 90-97% of the total mass of the anode active material, the conductive agent and the binder, and the lithium transition metal composite oxide is LiMxOy(ii) a LiMxOy is LiMn2O4、LiNiO2Or LiCoO2M is one or a combination of several transition metals.
The conductive agent is at least one of carbon black or conductive graphite; the binder is polyvinylidene fluoride; the solvent is NMP.
The negative electrode comprises a negative metal current collector, a negative active material, a conductive agent, a binder and a solvent; the negative metal current collector is copper foil, and the negative active material is at least one of lithium alloy, carbon, silicon carbon, petroleum coke, active carbon, graphite, carbon fiber or carbon nano tube; the mass of the negative electrode active material accounts for 90-97% of the total mass of the negative electrode active material, the conductive agent and the binder; the lithium transition metal composite oxide is LiMxOy,LiMxOyIs LiMn2O4、LiNiO2、LiCoO2Or LiMxPO4At least one of; LiMxPO4Is LiFePO4Or LiVPO4At least one of; m is one or a combination of several transition metals.
The conductive agent is at least one of carbon black or conductive graphite; the binder is at least one of CMC, SBR or polyacrylic acid; the solvent is deionized water.
The diaphragm is a polyolefin microporous diaphragm or a non-woven fabric diaphragm; the diaphragm is coated with a ceramic coating or an organic coating; the ceramic coating is one of alumina or boehmite; the organic coating is an aramid fiber high-melting-point organic coating; the thickness of the coating is 5-40um, and the porosity is 25-50%.
The preparation method of the high-safety lithium ion battery comprises the following steps:
(1) and (3) positive electrode: dissolving 95.5% of nickel cobalt lithium manganate, 2.5% of conductive agent and 2% of polyvinylidene fluoride in N-methyl-2-pyrrolidone to prepare positive electrode slurry. Coating the slurry on an aluminum foil, drying, rolling, and die-cutting into 232 × 189 mm;
(2) negative electrode: dissolving 95.5% of graphite, 1% of conductive agent, 1.5% of CMC and 2% of SBR in deionized water to prepare negative electrode slurry, coating the slurry on an aluminum foil, drying, rolling, and die-cutting into 236 x 192 mm;
(3) a diaphragm: the membrane comprises a polyolefin substrate and a double-sided alumina coating membrane, and the thickness of the membrane is 16+2+2 um;
(4) and laminating and encapsulating the positive electrode, the negative electrode and the diaphragm in an aluminum plastic film, and performing processes of liquid injection, pre-charging and the like to prepare the battery.
Compared with the prior art, the high-safety electrolyte and the lithium ion battery thereof have the following advantages:
(1) the high-safety electrolyte contains an inorganic film-forming agent and a long-chain organic film-forming agent, and a graphite-thin inorganic SEI film-loose thick organic SEI film mode is formed by controlling the molecular structure of the film-forming agent and matching with a proper pre-charging system, so that the electronic impedance of a negative electrode is increased, and the safety of a battery is improved; long-chain additives are used, so that the film thickness is only increased, lithium ions are not consumed too much, and the capacity is ensured; the electronic impedance of the cathode is increased, the reduction reaction of the electrolyte solvent on the surface of the cathode is reduced, the self-discharge is reduced, and the cycle performance is ensured; the organic SEI film is in a loose structure, so that the power performance is not obviously reduced; the organic film has long molecular chain, the formed SEI film is more difficult to decompose, and the side reaction in the battery is less.
(2) The high-safety electrolyte disclosed by the invention is added with the film forming agent, and compared with the reagent I, the reagent II is added with a carbon-oxygen bond, so that the molecular toughness is improved, and the cracking of an SEI film during the charge-discharge expansion of a negative electrode can be reduced.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Example 1
A high-safety electrolyte comprises 3% of reagent I (n is 4), 3:7 of EC and EMC, and 1.15M of LiPF62% of VC and 1% of lithium difluorophosphate.
A high-safety lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm and the electrolyte.
The pre-charging temperature of the electrolyte is 10-100 ℃; the thickness of the pre-charged SEI film is more than or equal to 40 nm.
The preparation method of the high-safety lithium ion battery comprises the following steps:
(1) and (3) positive electrode: dissolving 95.5% of nickel cobalt lithium manganate, 2.5% of conductive agent and 2% of polyvinylidene fluoride in N-methyl-2-pyrrolidone to prepare positive electrode slurry. Coating the slurry on an aluminum foil, drying, rolling, and die-cutting into 232 × 189 mm;
(2) negative electrode: dissolving 95.5% of graphite, 1% of conductive agent, 1.5% of CMC and 2% of SBR in deionized water to prepare negative electrode slurry, coating the slurry on an aluminum foil, drying, rolling, and die-cutting into 236 x 192 mm;
(3) a diaphragm: the membrane comprises a polyolefin substrate and a double-sided alumina coating membrane, and the thickness of the membrane is 16+2+2 um;
(4) electrolyte solution: mixing EC and EMC according to a volume ratio of 30:70, adding LiPF6 according to a lithium salt concentration of 1.15M, respectively adding 3% of I, 2% of VC and 1% of lithium difluorophosphate, and fully stirring to prepare an electrolyte;
(5) and laminating and encapsulating the positive electrode, the negative electrode and the diaphragm in an aluminum plastic film, and performing processes of liquid injection, pre-charging and the like to prepare the battery.
Example 2
A high-safety electrolyte comprises 4% of a reagent I (n is 10), 3:7 of EC and EMC, and 1.15M of LiPF62% of VC and 1% of lithium difluorophosphate.
A high-safety lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm and the electrolyte.
The pre-charging temperature of the electrolyte is 10-100 ℃; the thickness of the pre-charged SEI film is more than or equal to 40 nm.
The preparation method of the high-safety lithium ion battery comprises the following steps:
(1) and (3) positive electrode: dissolving 95.5% of nickel cobalt lithium manganate, 2.5% of conductive agent and 2% of polyvinylidene fluoride in N-methyl-2-pyrrolidone to prepare positive electrode slurry. Coating the slurry on an aluminum foil, drying, rolling, and die-cutting into 232 × 189 mm;
(2) negative electrode: dissolving 95.5% of graphite, 1% of conductive agent, 1.5% of CMC and 2% of SBR in deionized water to prepare negative electrode slurry, coating the slurry on an aluminum foil, drying, rolling, and die-cutting into 236 x 192 mm;
(3) a diaphragm: the membrane comprises a polyolefin substrate and a double-sided alumina coating membrane, and the thickness of the membrane is 16+2+2 um;
(4) electrolyte solution: mixing EC and EMC according to a volume ratio of 30:70, adding LiPF6 according to a lithium salt concentration of 1.15M, respectively adding 3% of I, 2% of VC and 1% of lithium difluorophosphate, and fully stirring to prepare an electrolyte;
(5) and laminating and encapsulating the positive electrode, the negative electrode and the diaphragm in an aluminum plastic film, and performing processes of liquid injection, pre-charging and the like to prepare the battery.
Example 3
A highly safe electrolyte solution comprising 3% of reagent II (n-3), 3:7 EC and EMC, and 1.15M LiPF62% of VC and 1% of lithium difluorophosphate.
A high-safety lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm and the electrolyte.
The pre-charging temperature of the electrolyte is 10-100 ℃; the thickness of the pre-charged SEI film is more than or equal to 40 nm.
The preparation method of the high-safety lithium ion battery comprises the following steps:
(1) and (3) positive electrode: dissolving 95.5% of nickel cobalt lithium manganate, 2.5% of conductive agent and 2% of polyvinylidene fluoride in N-methyl-2-pyrrolidone to prepare positive electrode slurry. Coating the slurry on an aluminum foil, drying, rolling, and die-cutting into 232 × 189 mm;
(2) negative electrode: dissolving 95.5% of graphite, 1% of conductive agent, 1.5% of CMC and 2% of SBR in deionized water to prepare negative electrode slurry, coating the slurry on an aluminum foil, drying, rolling, and die-cutting into 236 x 192 mm;
(3) a diaphragm: the membrane comprises a polyolefin substrate and a double-sided alumina coating membrane, and the thickness of the membrane is 16+2+2 um;
(4) electrolyte solution: mixing EC and EMC according to a volume ratio of 30:70, adding LiPF6 according to a lithium salt concentration of 1.15M, respectively adding 3% of I, 2% of VC and 1% of lithium difluorophosphate, and fully stirring to prepare an electrolyte;
(5) and laminating and encapsulating the positive electrode, the negative electrode and the diaphragm in an aluminum plastic film, and performing processes of liquid injection, pre-charging and the like to prepare the battery.
Example 4
A high-safety electrolyte contains 4% of reagent II (n is 8), 3:7 EC and EMC, and 1.15M LiPF62% of VC and 1% of lithium difluorophosphate.
A high-safety lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm and the electrolyte.
The pre-charging temperature of the electrolyte is 10-100 ℃; the thickness of the pre-charged SEI film is more than or equal to 40 nm.
The preparation method of the high-safety lithium ion battery comprises the following steps:
(1) and (3) positive electrode: dissolving 95.5% of nickel cobalt lithium manganate, 2.5% of conductive agent and 2% of polyvinylidene fluoride in N-methyl-2-pyrrolidone to prepare positive electrode slurry. Coating the slurry on an aluminum foil, drying, rolling, and die-cutting into 232 × 189 mm;
(2) negative electrode: dissolving 95.5% of graphite, 1% of conductive agent, 1.5% of CMC and 2% of SBR in deionized water to prepare negative electrode slurry, coating the slurry on an aluminum foil, drying, rolling, and die-cutting into 236 x 192 mm;
(3) a diaphragm: the membrane comprises a polyolefin substrate and a double-sided alumina coating membrane, and the thickness of the membrane is 16+2+2 um;
(4) electrolyte solution: mixing EC and EMC according to a volume ratio of 30:70, adding LiPF6 according to a lithium salt concentration of 1.15M, respectively adding 3% of I, 2% of VC and 1% of lithium difluorophosphate, and fully stirring to prepare an electrolyte;
(5) and laminating and encapsulating the positive electrode, the negative electrode and the diaphragm in an aluminum plastic film, and performing processes of liquid injection, pre-charging and the like to prepare the battery.
Comparative example 1
An electrolyte comprises EC and EMC of 3:7 and LiPF of 1.15M62% of VC and 1% of lithium difluorophosphate.
A high-safety lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm and the electrolyte.
The preparation method of the lithium ion battery comprises the following steps:
(1) and (3) positive electrode: dissolving 95.5% of nickel cobalt lithium manganate, 2.5% of conductive agent and 2% of polyvinylidene fluoride in N-methyl-2-pyrrolidone to prepare positive electrode slurry. Coating the slurry on an aluminum foil, drying, rolling, and die-cutting into 232 × 189 mm;
(2) negative electrode: dissolving 95.5% of graphite, 1% of conductive agent, 1.5% of CMC and 2% of SBR in deionized water to prepare negative electrode slurry, coating the slurry on an aluminum foil, drying, rolling, and die-cutting into 236 x 192 mm;
(3) a diaphragm: the membrane comprises a polyolefin substrate and a double-sided alumina coating membrane, and the thickness of the membrane is 16+2+2 um;
(4) electrolyte solution: mixing EC and EMC according to a volume ratio of 30:70, adding LiPF6 according to a lithium salt concentration of 1.15M, respectively adding 2% of VC and 1% of lithium difluorophosphate, and fully stirring to prepare electrolyte;
(5) and laminating and encapsulating the positive electrode, the negative electrode and the diaphragm in an aluminum plastic film, and performing processes of liquid injection, pre-charging and the like to prepare the battery.
The lithium ion batteries obtained in examples 1 to 4 and comparative example 1 were tested:
1. recording the first discharge capacity of the battery and the DCR of 2C;
2. the Transmission Electron Microscope (TEM) was used to test the average thickness of the SEI film after compatibilization;
3. the battery was tested for needle safety. The cell was charged at 1C to 4.2V, 0.05C. The high-temperature resistant steel needle with the diameter of 8mm penetrates through the battery pole piece from the direction vertical to the battery pole piece at the speed of (25 +/-5) mm/S. The steel needle was left in the cell and observed for 1 h. Test 3 replicates;
4. storage test at 25 ℃. The cell was charged to 4.2V,0.05C at 1C for 30min, then discharged to 2.75V at 1C for 30min, and then charged to 4.2V,0.05C at 1C. And recording the discharge capacity, voltage and internal resistance of the battery before storage. The battery was left to stand at (25. + -. 3) ℃ for 30 days. And recording the stored voltage and internal resistance of the battery. The cell was discharged to 2.75V at 1C current, left to stand for 30min, then charged to 4.2V,0.05C at 1C, and then discharged to 2.75V at 1C, and the cell discharge capacity after storage was recorded. Test 3 replicates;
5. and (4) cycle performance. The cycling test was carried out in an oven at (45 + -2) ° C under the conditions of 1C/1C, and the charge-discharge cutoff conditions were 4.2V,0.05C and 2.75V.
The test results are shown in table 1.
TABLE 1 test results
From the test results, the battery can be needled, the storage performance is improved, the capacity and the cycle performance are not greatly different from those of the comparative example, and the DCR growth value is acceptable.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A high-safety electrolyte is characterized in that: the electrolyte comprises an organic film-forming agent; the organic film forming agent is at least one of an agent I or an agent II;
the structural formula of the reagent I is as follows:
the structural formula of the reagent II is as follows:
2. the high-safety electrolyte as claimed in claim 1, wherein: n is1=1-5;n2=1-5。
3. The high-safety electrolyte as claimed in claim 1, wherein: the addition amount of the organic film forming agent is 0.5-5%.
4. The high-safety electrolyte as claimed in claim 3, wherein: the electrolyte also comprises an electrolyte solvent, an electrolyte lithium salt and an inorganic film-forming agent;
the electrolyte solvent, the electrolyte lithium salt and the inorganic film-forming agent are as follows in parts by mass:
72-94 parts of an electrolyte solvent,
6-18 parts of lithium salt of the electrolyte,
0.5-5 parts of inorganic film forming agent.
5. The high-safety electrolyte as claimed in claim 3, wherein: the electrolyte solvent is a combination of cyclic carbonate and chain carbonate; the cyclic carbonate is at least one of ethylene carbonate, propylene carbonate, butylene carbonate, alpha-butyrolactone or alpha-valerolactone; the chain carbonate is at least one of dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, diethoxyethane or 1, 3-dioxolane.
6. The high-safety electrolyte as claimed in claim 3, wherein: the lithium salt of the electrolyte is LiPF6、LiBF4、LiClO4、LiBOB、LiN(CF3SO2)2Or Li (CF)3SO2)3At least one of; the concentration of the lithium salt of the electrolyte is 0.5-1.5M.
7. The high-safety electrolyte as claimed in claim 3, wherein: the inorganic film-forming agent is at least one of lithium difluorophosphate, vinylene carbonate or propylene sulfite.
8. A high-safety lithium ion battery is characterized in that: the lithium ion battery comprises a positive electrode, a negative electrode, a separator and the electrolyte of any one of claims 1 to 6.
9. The high-safety lithium ion battery according to claim 7, wherein: the pre-charging temperature of the electrolyte is 10-100 ℃; the thickness of the pre-charged SEI film is more than or equal to 40 nm.
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