CN113659214B - Design method of high specific energy lithium ion battery with electrochemical performance and safety performance - Google Patents
Design method of high specific energy lithium ion battery with electrochemical performance and safety performance Download PDFInfo
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000013461 design Methods 0.000 title claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 64
- 238000011156 evaluation Methods 0.000 claims abstract description 17
- 239000010405 anode material Substances 0.000 claims abstract description 14
- 230000000694 effects Effects 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 230000003647 oxidation Effects 0.000 claims abstract description 5
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 15
- 239000007774 positive electrode material Substances 0.000 claims description 11
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000012795 verification Methods 0.000 claims description 5
- 229910013716 LiNi Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052744 lithium Inorganic materials 0.000 abstract description 7
- 239000010406 cathode material Substances 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 4
- 238000012827 research and development Methods 0.000 abstract description 4
- 238000012216 screening Methods 0.000 abstract 1
- 239000003792 electrolyte Substances 0.000 description 6
- -1 Polyethylene Polymers 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 4
- 229920000573 polyethylene Polymers 0.000 description 4
- 229920001155 polypropylene Polymers 0.000 description 4
- 239000011572 manganese Substances 0.000 description 3
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical group O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 2
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- QFJXEGDEAHXTDK-UHFFFAOYSA-N 1,2,3-trifluoro-4-phenylbenzene Chemical group FC1=C(F)C(F)=CC=C1C1=CC=CC=C1 QFJXEGDEAHXTDK-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 238000009783 overcharge test Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
- H01M10/058—Construction or manufacture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
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- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/385—Arrangements for measuring battery or accumulator variables
- G01R31/3865—Arrangements for measuring battery or accumulator variables related to manufacture, e.g. testing after manufacture
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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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a design method of a high specific energy lithium ion battery with both electrochemical performance and safety performance, which comprises the following steps: selecting materials: selecting a material with redox activity under high voltage as a material to be evaluated; preparation: preparing a lithium ion button cell taking the material to be evaluated as a positive electrode; evaluation: verifying the button cell, and evaluating the oxidation capacity and electrochemical performance of the material to be evaluated; material taking: and preferably obtaining the cathode material with both electrochemical performance and safety performance from a plurality of materials to be evaluated. According to the method, the screening of the battery anode is carried out by utilizing the high-voltage redox activity and gas production behavior of the anode material, so that the overcharge temperature rise is controlled within a certain range, and the overcharge safety performance of the lithium battery is improved; meanwhile, the overcharge safety performance of the anode material can be evaluated quickly, the research and development efficiency is improved, and the development cost is saved.
Description
Technical Field
The invention relates to the field of lithium batteries, in particular to the design of a lithium battery.
Background
With the application of a large amount of cathode materials with higher and higher nickel content to lithium ion batteries, the energy density of lithium batteries is rapidly improved, but the safety problems such as thermal runaway and the like are more prominent. The positive electrode material, particularly the high-nickel positive electrode material, is unstable in structure in a high-potential and high-delithiation state, and easily releases oxygen and generates heat. The anode material in a high lithium removal state is easy to have violent side reaction with organic electrolyte to release a large amount of heat, so that the temperature of the battery is rapidly increased. The temperature rise will further promote the decomposition of the positive electrode material, aggravate the exothermic side reaction and finally cause thermal runaway. Especially, under the condition of electricity abuse, such as overcharge, the battery core is easy to explode and catch fire and other safety accidents.
In actual production, the lithium ion cathode material has wide sources, and a plurality of materials have different performances. The safety performance evaluation of the material can be carried out only after the material is made into a full battery, and challenges are brought to battery development work in aspects of time efficiency, manpower, material resources, resources and the like. And improving the research and development efficiency, and reducing the financial cost, the time cost and the labor cost have important significance for enterprises.
At present, the overcharge of the battery is mostly still limited on the level of introducing the overcharge-preventing additive, for example, in patent CN201410275652.6, 2,3,4-trifluorobiphenyl is added into the electrolyte, which forms a layer of dense electric insulating film on the positive electrode, prevents the battery active material and the electrolyte from being further oxidized, and improves the over-charge bearing capacity of the lithium battery.
Disclosure of Invention
The main purposes of the invention are: the problems of low development efficiency and difficult consideration of electrochemical performance and safety performance of the lithium ion battery in the prior art are solved.
Therefore, the invention provides a design method of a high specific energy lithium ion battery with both electrochemical performance and safety performance, which comprises the following steps:
selecting materials: selecting a material with redox activity under high voltage as a material to be evaluated;
preparation: preparing a lithium ion button cell taking the material to be evaluated as a positive electrode;
evaluation: verifying the button cell, and evaluating the oxidation capacity and the electrochemical performance of the material to be evaluated;
material taking: preferably obtaining a positive electrode material with both electrochemical performance and safety performance from the materials to be evaluated;
manufacturing a full cell: adopting the optimized positive electrode material with both electrochemical performance and safety performance to manufacture a lithium ion full battery;
and (3) verification: and verifying electrochemical performance and safety performance by adopting the lithium ion full battery.
In an optional embodiment of the above method for designing a high specific energy lithium ion battery with electrochemical performance and safety performance, the evaluating step includes:
1) Overcharging the lithium ion button cell to 6V or above at room temperature or high temperature of 45-80 ℃;
2) Collecting a voltage V-time t curve to obtain a differential curve dV/dt;
3) And comparing the voltage increase rates of the sample to be detected and the known sample, and judging the overcharge temperature rise and the gas production rate of the anode material.
According to the method, the redox activity and gas production behavior of the anode material under high voltage are evaluated, and the anode of the battery is screened, so that the overcharge temperature rise is controlled within a certain range, and the overcharge safety performance of the lithium battery is improved; the overcharge-preventing additive is not needed to be adopted for the anode material, so that the research and development cost of the battery can be reduced, and the safety performance of the battery can be ensured.
In the optional mode, the material to be evaluated is used as the anode material to prepare the lithium ion button cell, so that the overcharge safety performance of the anode material can be evaluated quickly, the material can be selected quickly, the research and development efficiency is improved, and the development cost is saved.
Drawings
FIG. 1 is a graph of cycle life for two materials in an example of the invention;
FIG. 2 is a plot of charging overcharge voltage V-time t for two materials in an embodiment of the invention;
FIG. 3 is a plot of the pinch overcharge voltage differential dV/dt versus time t for two materials in an example embodiment of the invention;
FIG. 4 is a temperature rise curve of the over-charge of the full cell in the embodiment of the present invention
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings. In some instances, certain operations related to the present application have not been shown or described in this specification in order not to obscure the core of the present application with unnecessary detail, and it is not necessary for those skilled in the art to describe these operations in detail, so that they may be fully understood from the description in the specification and the general knowledge in the art.
The invention relates to a design method of a high specific energy lithium ion battery with electrochemical performance and safety performance, which mainly comprises the following steps:
selecting materials: taking a material with redox activity under high voltage as a material to be evaluated;
preparation: preparing a button cell taking the material to be evaluated as a positive electrode;
evaluation: verifying the button cell, and evaluating the oxidation capacity and electrochemical performance of the material to be evaluated;
material taking: preferably obtaining a positive electrode material with both electrochemical performance and safety performance from the materials to be evaluated;
manufacturing a full cell: manufacturing a lithium ion full battery by adopting a positive electrode material which has both electrochemical performance and safety performance;
and (3) verification and evaluation: verifying electrochemical performance and safety performance by using a lithium ion full battery;
and (3) comparison: and comparing the evaluation result of the button cell with the evaluation result of the full cell for research.
Example one
Selecting materials: selecting material with redox activity under high voltage and LiNi with layered molecular formula x Co y M (1-x-y) O 2 ，1>x≥ 0.8，y<0.1, M is Mn, V, ru, mo, etc., and has redox activity at high voltage or a certain oxygen release capacity. For example, a high nickel material rich in manganese has a certain anionic redox reaction in a manganese-rich region under high voltage, while molybdenum has a higher redox valence state.
Preparation: preparing a lithium ion button cell, and activating for 2-3 weeks to ensure that the electrochemical performance of the lithium ion button cell is stable;
evaluation: verifying the lithium ion button cell, and evaluating the oxidation capacity and electrochemical performance of the material to be evaluated:
the lithium ion button cell is overcharged to more than 6V at room temperature or high temperature of 45-80 ℃;
collecting a voltage V-time t curve to obtain a differential curve dV/dt;
and comparing the voltage increase rates of the sample to be detected and the known sample, and judging the overcharge temperature rise and the gas production rate of the anode material. For example, in an alternative embodiment of this example, the lithium-ion button cell is in the form of a cylindrical cell, the cap of which has a CID structure, with an explosion pressure of 1.8-2.5MPa, plus the residual volume of the cylinder being a fixed value. During the battery overcharge experiment, the CID is opened and powered off by the generated gas; the over-charge time and the temperature are used for judging the gas generation speed, because the high voltage has strong decomposition effect on the electrolyte and temperature rise effect, different anode materials have different responses to the over-charge time and the temperature, and accordingly, the anode material which can give consideration to the safety performance can be preferably selected from various anode materials to be evaluated and used for the full-cell.
In order to improve the evaluation accuracy, the more suitable evaluation material emits a capacity difference of between 10 and 20 percent compared with the known material under the same voltage window, belongs to a homologous compound, and the electrochemical properties of the two are equivalent, including rated voltage, rated capacity, 1C capacity, high and low temperature properties, cycle life and the like, such as high nickel series, for example, similar specific capacity and crystal structure.
The lithium ion button cell battery comprises a positive electrode, a negative electrode, a diaphragm and electrolyte. The negative electrode of the lithium ion battery is graphite or a silicon compound, and the overcharge charging current of the lithium ion battery is within the current multiplying power use range specified by the battery. Each type of battery has its own current usage specification, such as energy type, power type, etc., with different current usage ranges.
The overcharge charging voltage of the lithium ion button cell battery is larger than the practical use upper limit voltage of the battery, the upper limit use voltage of the whole battery is generally 4.2 +/-0.05V, and the overcharge voltage is generally more than or equal to 6V.
This full battery of lithium ion possesses prior art's current cutting device, and when electric core became invalid, the battery was inside can produce a lot of gas, made the increase of battery internal pressure, and the solder joint that causes to weld on aluminum plate and the pressure release piece drops, and the pressure release piece upset leads to inside the opening circuit of electric core, and plays the guard action. Such as 18650, 21700, 26650 and 32105 for cylindrical batteries, 2614891, 3914895 and 5214895 for prismatic batteries.
Collecting and recording a voltage V-time t curve; when V is greater than 4.5V, if the voltage increase rate is higher, the voltage of the material to be evaluated is increased faster in the later stage of overcharge, the temperature is also increased faster, and the risk of thermal runaway brought to the battery is higher when the temperature of overcharge is higher.
Material taking: according to the verification of the lithium ion button cell, various materials to be evaluated are compared, and a stable material to be evaluated with electrochemical performance and safety performance compared is selected as a positive electrode material.
Example two
Referring to and combining the solution of the first embodiment, this embodiment specifically includes:
selecting materials: selecting a positive electrode material B (LiNi) to be evaluated 0.8 Co 0.05 M 0.15 O 2 ) The sample cathode material A (LiNi) has a constant ability to oxidize anionic oxygen at a high pressure under normal temperature conditions 0.8 Co 0.1 Al 0.1 O 2 ) And basically has no high-voltage oxidation-reduction capability. At high temperatures, both oxygen activities are enhanced, as is the case with the known samples. Both are high nickel materials, the nickel content is more than 80%, and the high nickel material has similar and higher specific capacity and similar crystal structure; it is known that the electrochemical performance of the two batteries is similar and excellent, and the cycle life curves of the two batteries are shown in the following figure 1.
The cell was prepared as follows: the diaphragm used for preparing the button cell is made of Polyethylene (PE) or polypropylene (PP) with the diameter of 16 microns; the electrolyte comprises ethylene carbonate EC, dimethyl carbonate DMC and diethyl carbonate DEC in a certain proportion, and the additive is vinylene carbonate VC and the like; and (3) activating the button cell for 3 weeks in a normal voltage window at normal temperature to stabilize the capacity of the cell.
Their thermal safety characteristics were evaluated. The temperature environment used for evaluation included normal temperature and high temperature. The reason for the high temperature is: in an actual use scene, the battery is continuously charged and discharged or an extremely high temperature scene occurs, so that the high temperature environment of 45-80 ℃ can be used as one of the evaluation environments. The voltage range is adjustable according to national standards or requirements, the upper line cut-off voltage is greater than 6V, and the optimal voltage is recommended to be 6V. Firstly, because the voltage of the ternary anode material is difficult to reach more than 6V, and secondly, the high-voltage test system with the measuring range of 6V is more common in consideration of the cost of the test instrument.
FIG. 2 shows the collected voltage V-time t curve of the battery, and accordingly the voltage derivative dV/dt-time t curve shown in FIG. 3 is obtained; when the battery voltage V>At 4.5V, its voltage increase rate dV A /t>dV B T; it shows that the voltage of the material a rises faster, the temperature rises faster and the temperature of overcharge is higher in the late stage of overcharge.
Preparing a lithium ion full battery: the used diaphragm polyethylene PE or polypropylene PP is 16 microns; the electrolyte consists of ethylene carbonate EC, dimethyl carbonate DMC and diethyl carbonate DEC in a certain proportion, and the additive is vinylene carbonate VC and the like.
And (3) verification and evaluation: performing 1C/12V adiabatic overcharge test on the lithium ion full cells of the known material A and the material B to be evaluated to obtain a temperature rise curve shown in figure 4, wherein the full cell voltage of the known material A is higher than the voltage of the material B to be evaluated in the later stage of overcharge, has a higher growth rate and is consistent with the lithium ion button cell result; and the time for the material A to reach the voltage peak is known to be long, the high voltage platform is delayed, and the overcharge temperature of the material A is also known to be higher than the temperature of the material B to be evaluated by about 20 ℃.
And (3) comparison: and comparing and researching the evaluation result of the button cell with the evaluation result of the full cell, and proving the feasibility of the evaluation principle again. The temperature of the battery with high voltage and high increasing speed in the later overcharge period is increased quickly, the temperature rise is higher, and the risk of thermal runaway brought to the battery is higher. Especially in the module overcharge scene, high temperature can lead to the temperature of module to be higher, makes the module more dangerous.
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. For a person skilled in the art to which the invention pertains, several simple deductions, modifications or substitutions may be made according to the idea of the invention.
Claims (5)
1. A design method of a high specific energy lithium ion battery with both electrochemical performance and safety performance comprises the following steps:
selecting materials: selecting a material with redox activity under high voltage as a material to be evaluated;
preparation: preparing a lithium ion button cell taking the material to be evaluated as a positive electrode;
evaluation: verifying the lithium ion button cell, and evaluating the oxidation capacity and electrochemical performance of the material to be evaluated;
material taking: preferably obtaining a positive electrode material with both electrochemical performance and safety performance from the multiple materials to be evaluated;
manufacturing a full cell: adopting the optimized positive electrode material with both electrochemical performance and safety performance to manufacture a lithium ion full battery;
and (3) verification: verifying electrochemical performance and safety performance by adopting the lithium ion full battery; the evaluating step includes:
1) Overcharging the lithium ion button cell to 6V or above 6V at room temperature or high temperature of 45-80 ℃;
2) Collecting a voltage V-time t curve to obtain a differential curve dV/dt;
3) And comparing the voltage increase rates of the lithium ion button cell and a known sample, and judging the overcharge temperature rise and the gas production rate of the anode material.
2. The method according to claim 1, wherein the method comprises the following steps: the material with redox activity under high voltage has LiNi with a molecular formula of a laminated structure x Co y M (1-x-y) O 2 ，1>x≥0.8，y<0.1, M is a metal element having redox activity or having oxygen-releasing ability at a high voltage.
3. The method according to claim 2, wherein the method comprises the following steps: the difference of the capacities of the material to be evaluated and the known material of the known sample is within the range of 10-20% under the same voltage window, the material to be evaluated and the known material of the known sample are both high nickel materials, and the nickel content is more than 80%.
4. The method for designing a high specific energy lithium ion battery with electrochemical performance and safety performance as claimed in claim 2 or 3, wherein: and M is one of Mn, V, ru or Mo.
5. The method for designing a high specific energy lithium ion battery having electrochemical properties and safety as claimed in claim 2 or 3, wherein: the lithium ion full battery is provided with a current cut-off device and is used for internal open circuit when internal pressure is increased due to failure of a battery cell, so that a protection effect is achieved.
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| CN107394193A (en) * | 2017-06-30 | 2017-11-24 | 湖南金富力新能源股份有限公司 | Anode material for lithium-ion batteries and its preparation method and application |
| CN111965204A (en) * | 2020-08-14 | 2020-11-20 | 厦门厦钨新能源材料股份有限公司 | Method for evaluating electrical activity of lithium ion battery anode material |
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