CN115312717A - Low-temperature-resistant lithium ion battery negative electrode slurry and preparation method and application thereof - Google Patents
Low-temperature-resistant lithium ion battery negative electrode slurry and preparation method and application thereof Download PDFInfo
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- H01—ELECTRIC ELEMENTS
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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
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
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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
- H01M4/00—Electrodes
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention discloses low-temperature-resistant lithium ion battery negative electrode slurry and a preparation method and application thereof, and belongs to the technical field of lithium ion batteries. The low-temperature-resistant lithium ion battery cathode slurry consists of the following components in percentage by mass: 42 to 48.5 percent of negative electrode material, 0.1 to 3.0 percent of polyacrylate adhesive, 1 to 2.0 percent of conductive agent, 0.6 to 1.5 percent of sodium carboxymethyl cellulose and 45 to 55 percent of deionized water. The cathode slurry can improve the compatibility of the electrolyte and the cathode material at low temperature, improve the ion transfer rate, reduce the internal resistance and effectively ensure the low-temperature discharge performance of the lithium ion battery.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to low-temperature-resistant lithium ion battery cathode slurry and a preparation method and application thereof.
Background
The working principle of the lithium ion battery is as follows: li + Diffusion in electrolyte by charge transfer and Li + The mutual conversion of electric energy and chemical energy is realized by embedding and releasing on the positive electrode and the negative electrode. Along with the rapid development of the electronic cigarette industry, the low-temperature resistance of the electronic cigarette batteryThe demand is higher and higher, and the low-temperature performance of lithium ion batteries is influenced by Li + Rate of motion in positive and negative electrode materials, li + The rate of movement in the electrolyte, the electrolyte/electrolyte interface film resistance, the rate of charge transfer, and the like. At present, most of electrolytes on the market have increased viscosity in a low-temperature environment, so that the ion transfer rate is reduced; even the solvent component crystallizes at a low temperature, resulting in an increase in the internal resistance of the battery and a decrease in the discharge efficiency.
Therefore, it is necessary to develop a low temperature resistant lithium ion battery negative electrode slurry and a preparation method thereof, which can improve the compatibility of the electrolyte and the negative electrode material at low temperature, increase the ion transfer rate, and reduce the internal resistance, so as to solve the problems that the existing lithium ion battery is difficult to transport and store at low temperature and difficult to discharge at low temperature.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the low-temperature-resistant lithium ion battery negative electrode slurry and the preparation method thereof.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the low-temperature-resistant lithium ion battery cathode slurry comprises the following components in percentage by mass: 42 to 48.5 percent of negative electrode material, 0.1 to 3.0 percent of polyacrylate adhesive, 1 to 2.0 percent of conductive agent, 0.6 to 1.5 percent of sodium carboxymethyl cellulose and 45 to 55 percent of deionized water.
In a preferred embodiment of the present invention, the negative electrode material is one of artificial graphite, natural graphite, lithium titanate, a lithium alloy, and nano silicon carbon powder.
In a preferred embodiment of the present invention, the conductive agent is one of conductive carbon black, carbon nanotubes, graphene, and carbon fibers.
The second purpose of the present invention is to provide a preparation method of the above low temperature resistant lithium ion battery negative electrode slurry, which specifically comprises the following steps:
s1, mixing sodium carboxymethylcellulose with a formula amount and part of deionized water, and uniformly stirring to form a first glue solution;
s2, adding the negative electrode material in the formula amount into the first glue solution, and uniformly stirring to form a second glue solution;
s3, adding the conductive agent and the rest deionized water in the formula amount into the second glue solution, and uniformly stirring to obtain a third glue solution;
s4, adding a polyacrylate adhesive into the third glue solution, controlling the solid content to be 44-48%, uniformly stirring, and vacuumizing to obtain a slurry;
and S5, defoaming the obtained slurry, and charging air to discharge vacuum to obtain the lithium ion battery cathode slurry.
In a preferred embodiment of the present invention, the degree of vacuum in the step S4 is-0.08 MPa.
The invention also aims to provide a low-temperature-resistant lithium ion battery, which comprises a positive pole piece, a negative pole piece made of the negative pole slurry, a diaphragm and low-temperature electrolyte.
As a preferred embodiment of the present invention, the low-temperature electrolyte comprises the following components in percentage by mass: electrolyte salt 10-15 wt%, non-water organic solvent 73-88 wt% and additive 1-12 wt%.
As a preferred embodiment of the present invention, the electrolyte salt is a mixture of lithium tetrafluoroborate and lithium bis (oxalato) borate.
As a preferred embodiment of the present invention, the non-aqueous organic solvent is at least one selected from the group consisting of ethyl acetate, ethylene carbonate, propylene carbonate, and ethyl methyl carbonate.
As a preferred embodiment of the present invention, the additive is at least one selected from triphenyl phosphate, ethylene monofluoromethyl carbonate, ethylene difluoromethyl carbonate, or ethylene trifluoromethylcarbonate.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the polyacrylic acid binder is added into the negative electrode slurry, so that a good solid electrolyte interface layer can be formed on the surface of the negative electrode, the compatibility of the low-temperature electrolyte and the negative electrode material can be improved, meanwhile, the strong adhesive force between the negative electrode material and the current collector is ensured, and the mechanical property of the pole piece is improved. In addition, by optimizing the proportion of the low-temperature electrolyte and combining the negative electrode slurry disclosed by the invention, the ion transfer rate of the prepared lithium ion battery is improved, the internal resistance is reduced, the lithium ion battery is convenient to transport and store in alpine regions, the rate discharge capacity can be quickly recovered at minus 10 ℃, the low-temperature storage performance and the low-temperature rate discharge performance of the lithium ion battery are improved, and therefore the problems that the battery is difficult to transport, store and discharge at low temperature are solved.
Drawings
Fig. 1 is a low-temperature discharge performance test curve of a lithium ion battery provided in embodiment 2 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the drawings and the detailed description.
The low-temperature-resistant lithium ion battery negative electrode slurry comprises the following components in percentage by mass: 42 to 48.5 percent of negative electrode material, 0.1 to 3.0 percent of polyacrylate adhesive, 1 to 2.0 percent of conductive agent, 0.6 to 1.5 percent of sodium carboxymethyl cellulose and 45 to 55 percent of deionized water. Wherein the negative electrode material is one of artificial graphite, natural graphite, lithium titanate, lithium alloy and nano silicon carbon powder; the conductive agent is one of conductive carbon black, carbon nano tubes, graphene and carbon fibers. The preparation method comprises the following steps:
s1, mixing sodium carboxymethylcellulose with a formula amount and part of deionized water, stirring for 5-10 min at a revolution speed of 5r/min and a rotation speed of 200r/min, and stirring for 120min at a revolution speed of 35r/min and a rotation speed of 1700r/min to form a first glue solution;
s2, adding a negative electrode material with a formula amount into the first glue solution, and stirring for 120min at a rotating speed of revolution of 35r/min and rotation of 1700r/min to form a second glue solution;
s3, adding the conductive agent and the rest deionized water in the formula amount into the second glue solution, and stirring for 90min at the rotating speed of revolution of 35r/min and rotation of 1700r/min to obtain a third glue solution;
s4, adding a polyacrylate adhesive into the third glue solution, controlling the solid content to be 44-48%, stirring for 30min at a revolution speed of 25r/min and a rotation speed of 900r/min, vacuumizing to obtain slurry at a vacuum degree of-0.08 MPa;
and S5, defoaming the obtained slurry, and charging air to discharge vacuum to obtain the lithium ion battery cathode slurry.
A low-temperature-resistant lithium ion battery comprises a positive pole piece, a negative pole piece made of the negative pole slurry, a diaphragm and low-temperature electrolyte. The low-temperature electrolyte comprises the following components in percentage by mass: electrolyte salt 10-15 wt%, non-water organic solvent 73-88 wt% and additive 1-12 wt%. The electrolyte salt is a mixture of lithium tetrafluoroborate and lithium bis (oxalato) borate. The non-aqueous organic solvent is at least one selected from ethyl acetate, ethylene carbonate, propylene carbonate or ethyl methyl carbonate. The additive is at least one of triphenyl phosphate, monofluoromethyl ethylene carbonate, difluoro methyl ethylene carbonate or trifluoro methyl ethylene carbonate.
Example 1:
a low-temperature-resistant lithium ion battery comprises a negative pole piece and low-temperature electrolyte.
The negative pole piece is made of low-temperature-resistant lithium ion battery negative pole slurry, and the negative pole slurry consists of the following components in percentage by mass: 43% of natural graphite, 1% of conductive carbon black, 1% of sodium carboxymethylcellulose (CMC), 54.9% of deionized water and 0.1% of polyacrylate adhesive.
The preparation method of the anode slurry comprises the following steps:
s1, mixing sodium carboxymethylcellulose with a formula amount and partial deionized water, firstly stirring at a rotating speed of revolution of 5r/min and rotation of 200r/min for 5-10 min, and then stirring at a rotating speed of revolution of 35r/min and rotation of 1700r/min for 120min to form a first glue solution;
s2, adding a negative electrode material with a formula amount into the first glue solution, and stirring for 120min at a rotating speed of revolution of 35r/min and rotation of 1700r/min to form a second glue solution;
s3, adding the conductive agent and the rest deionized water in the formula amount into the second glue solution, and stirring for 90min at the rotating speed of revolution of 35r/min and rotation of 1700r/min to obtain a third glue solution;
s4, adding a polyacrylate adhesive into the third glue solution, controlling the solid content to be 45.4%, stirring for 30min at a revolution speed of 25r/min and a rotation speed of 900r/min, vacuumizing to enable the vacuum degree to be-0.08 MPa, and obtaining slurry;
and S5, defoaming the obtained slurry, and charging air to discharge vacuum to obtain the lithium ion battery cathode slurry.
The low-temperature electrolyte comprises the following components in percentage by mass: 10% of lithium tetrafluoroborate, 2% of lithium bis (oxalato) borate, 83% of nonaqueous organic solvent and 5% of triphenyl phosphate. Before preparation, the solid components are dried by using a 3A molecular sieve, so that the moisture content of the electrolyte is ensured to be below 150 ppm. The preparation process is as follows: mixing ethyl acetate, ethylene carbonate, propylene carbonate and methyl ethyl carbonate according to the mass ratio of 3. The preparation process is completed in a glove box filled with argon protective atmosphere.
Preparing a lithium ion battery: the negative electrode slurry is used for preparing the lithium ion battery through the steps of coating, rolling, stripping, flaking, winding, packaging, injecting, aging, formation, secondary sealing, capacity grading, full inspection and the like. Wherein, the electrolyte adopted for injection is the low-temperature electrolyte, and the weight proportion of the electrolyte in the battery is 25%.
Example 2:
a low-temperature-resistant lithium ion battery comprises a negative pole piece and low-temperature electrolyte. The present example differs from example 1 in that: the adopted low-temperature-resistant lithium ion battery cathode slurry consists of the following components in percentage by mass: 43% of natural graphite, 1% of conductive carbon black, 1% of sodium carboxymethylcellulose CMC, 53% of deionized water and 2% of polyacrylate adhesive. The rest was the same as in example 1.
The discharge performance of the lithium ion battery was measured at a normal temperature of 25 ℃ and a low temperature of-10 ℃ respectively, and the results are shown in fig. 1. As can be seen from fig. 1, the discharge platforms of the lithium ion battery prepared by the invention at low temperature of-10 ℃ and normal temperature are all 3.2V, the low-temperature discharge capacity is 659.8mAh, the normal-temperature discharge capacity is 789.2mAh, and the ratio of the low-temperature discharge capacity to the normal-temperature discharge capacity is 83%, so that the lithium ion battery prepared by the embodiment has good low-temperature discharge capacity.
Example 3:
a low-temperature-resistant lithium ion battery comprises a negative pole piece and low-temperature electrolyte. This example differs from example 1 in that: the adopted low-temperature-resistant lithium ion battery cathode slurry consists of the following components in percentage by mass: 43% of artificial graphite, 1% of graphene, 1% of sodium carboxymethylcellulose (CMC), 52% of deionized water and 3% of polyacrylate adhesive. The rest was the same as in example 1.
Comparative example 1:
the comparative example differs from example 2 in that: the electrolyte adopted in the electrolyte is different in electrolyte salt, and the specific composition is as follows: the normal-temperature electrolyte comprises the following components in percentage by mass: 12% of lithium hexafluorophosphate, 83% of a nonaqueous organic solvent and 5% of triphenyl phosphate. The rest of the procedure was the same as in example 1.
Comparative example 2:
this comparative example differs from example 1 in that: the adopted adhesive is Styrene Butadiene Rubber (SBR). The rest of the procedure was the same as in example 1.
Comparative example 3:
this comparative example differs from example 2 in that: the adopted adhesive is Styrene Butadiene Rubber (SBR). The rest was the same as in example 2.
Comparative example 4:
this comparative example differs from example 3 in that: the adopted adhesive is Styrene Butadiene Rubber (SBR). The rest was the same as in example 3.
Bond effect verification experiment:
the negative electrode sheets obtained in examples 1 to 3 and comparative examples 1 to 4 were tested for adhesion effect and mechanical strength of the sheet, and the results are shown in table 1.
TABLE 1 comparison of the results of adhesion and mechanical strength of examples 1-3 with comparative examples 1-4
| Item | Type and amount of binder | Pole piece bonding effect | Mechanical strength of pole piece |
| Example 1 | Polyacrylate 0.1% | Difference (D) | Difference (D) |
| Example 2 | Polyacrylate 2% | Youyou (an instant noodle) | Youyou (an instant noodle) |
| Example 3 | Polyacrylate 3% | Good effect | Good effect |
| Comparative example 1 | Polyacrylate 2% | Superior food | Youyou (an instant noodle) |
| Comparative example 2 | Styrene butadiene rubber 0.1% | Difference (D) | Difference (D) |
| Comparative example 3 | 2 percent of styrene-butadiene rubber | Good effect | Is good |
| Comparative example 4 | 3 percent of styrene-butadiene rubber | Good effect | Good effect |
As can be seen from the analysis of Table 1, the low addition ratio of the styrene-butadiene rubber or the polyacrylate adhesive leads to poor adhesion effect because the addition amount of the adhesive is small, so that the active material and the adhesive on the pole piece are not uniformly dispersed. When the addition proportion is 2%, the pole piece bonding effect of the polyacrylate is better than that of styrene butadiene rubber, because the polyacrylate adhesive can form a good solid electrolyte interface layer on the surface of the negative electrode at the proportion, the compatibility of the low-temperature electrolyte and the negative electrode material can be improved. When the polyacrylate is added in a proportion of 3%, the binding effect is reduced because the negative electrode slurry is difficult to disperse by stirring, and is liable to agglomerate. Therefore, the negative electrode slurry obtains better compatibility of the low-temperature electrolyte and the negative electrode material by selecting the specific polyacrylate adhesive and screening the dosage of the polyacrylate adhesive.
Low-temperature discharge performance verification experiment:
the lithium ion batteries prepared in examples 1 to 3 and comparative examples 1 to 4 were subjected to a low-temperature charge test, which specifically performed as follows: the lithium ion battery is charged with 1C constant current and constant voltage at normal temperature, the battery is placed in a low-temperature box at minus 10 +/-2 ℃ for standing for 4H, then discharged to 3.0V at the current of 3A, taken out, placed for 2H at the temperature of 25 +/-5 ℃, and the appearance is observed, and the result is shown in Table 2.
TABLE 2 comparison of test results of Low-temperature discharge Properties of examples 1 to 3 with comparative examples 1 to 4
Analysis of Table 2 shows that the internal resistances of examples 1-3 are lower than those of comparative examples 1-4, which indicates that the polyacrylate adhesive can effectively reduce the contact resistance, reduce the electrode polarization and improve the electrochemical performance by matching with the low-temperature electrolyte. After the test, the residual (discharge) capacity and the median voltage of the batteries of the examples 1 to 3 are higher than the corresponding ratio of 1 to 4, which shows that the thin and compact SEI film is formed on the negative electrode of the lithium ion battery prepared by the invention, and the Li is ensured + The active material has a larger diffusion coefficient, thereby ensuring the discharge capability of the battery at low temperature, and the battery does not deform, burst or leak liquid under low-temperature discharge and has good safety performance.
Low-temperature storage performance verification experiment:
the lithium ion batteries prepared in examples 1 to 3 and comparative examples 1 to 4 were subjected to a low temperature storage test, which specifically performed as follows: the cell was charged fully according to the standard, the voltage and internal resistance were recorded, 24H was set aside at-40 ± 2 ℃, the voltage and internal resistance were recorded, 3A was discharged to 3.0V after 2H was set aside at-10 ± 2 ℃, and the results are shown in table 3.
TABLE 3 comparison of test results of Low temperature storage Properties of examples 1 to 3 and comparative examples 1 to 4
As can be seen from Table 3, the lithium ion batteries of examples 1 to 3 had an internal resistance increase rate of not more than 5% and a voltage drop rate of not more than 1% after 24 hours of storage at-40. + -. 2 ℃ and no ballooning or liquid leakage, and could be well discharged at-10 ℃ while the lithium ion batteries of comparative examples 1 to 4 had an internal resistance increase rate of mostly more than 5% and a voltage drop rate of mostly more than 1%, and it was seen that the lithium ion batteries of examples 1 to 3 could be stored at-40 ℃.
In conclusion, the lithium ion battery provided by the invention adopts the polyacrylate adhesive to replace the original aqueous adhesive SBR, and the low-temperature storage performance and the low-discharge performance of the lithium ion battery prepared by adopting the low-temperature electrolyte are superior to those of the lithium ion battery prepared by adopting the SBR as the adhesive, and the lithium ion battery prepared by the invention can be stored at the temperature of minus 40 ℃ and can carry out 3A multiplying power discharge when the temperature is restored to the temperature of minus 10 ℃.
The above embodiments are only preferred embodiments of the present invention, and the scope of the present invention should not be limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
Claims (10)
1. The low-temperature-resistant lithium ion battery cathode slurry is characterized in that: the paint consists of the following components in percentage by mass: 42 to 48.5 percent of negative electrode material, 0.1 to 3.0 percent of polyacrylate adhesive, 1 to 2.0 percent of conductive agent, 0.6 to 1.5 percent of sodium carboxymethyl cellulose and 45 to 55 percent of deionized water.
2. The low temperature resistant lithium ion battery negative electrode slurry of claim 1, wherein: the negative electrode material is one of artificial graphite, natural graphite, lithium titanate, lithium alloy and nano silicon-carbon powder.
3. The low temperature resistant lithium ion battery negative electrode slurry of claim 1, wherein: the conductive agent is one of conductive carbon black, carbon nano tubes, graphene and carbon fibers.
4. A method for preparing the low temperature resistant lithium ion battery negative electrode slurry of any one of claims 1 to 3, characterized in that: the method comprises the following steps:
s1, mixing sodium carboxymethylcellulose with a formula amount and part of deionized water, and uniformly stirring to form a first glue solution;
s2, adding the negative electrode material in the formula amount into the first glue solution, and uniformly stirring to form a second glue solution;
s3, adding the conductive agent and the residual deionized water in the formula amount into the second glue solution, and uniformly stirring to obtain a third glue solution;
s4, adding a polyacrylate adhesive into the third glue solution, controlling the solid content to be 44-48%, uniformly stirring, and vacuumizing to obtain a slurry;
and S5, defoaming the obtained slurry, and charging air to discharge vacuum to obtain the lithium ion battery cathode slurry.
5. The preparation method of the low temperature resistant lithium ion battery negative electrode slurry according to claim 4, characterized in that: the vacuum degree in the step S4 is-0.08 MPa.
6. A low temperature resistant lithium ion battery is characterized in that: the lithium ion battery comprises a positive pole piece, a negative pole piece made of the negative pole slurry of any one of claims 1 to 3, a diaphragm and low-temperature electrolyte.
7. The low temperature resistant lithium ion battery of claim 6, wherein: the low-temperature electrolyte comprises the following components in percentage by mass: electrolyte salt 10-15 wt%, non-water organic solvent 73-88 wt% and additive 1-12 wt%.
8. The low temperature resistant lithium ion battery of claim 7, wherein: the electrolyte salt is a mixture of lithium tetrafluoroborate and lithium bis (oxalato) borate.
9. The low temperature resistant lithium ion battery of claim 7, wherein: the non-aqueous organic solvent is at least one selected from ethyl acetate, ethylene carbonate, propylene carbonate or ethyl methyl carbonate.
10. The low temperature resistant lithium ion battery of claim 7, wherein: the additive is at least one of triphenyl phosphate, ethylene monofluoromethyl carbonate, ethylene difluoromethyl carbonate or ethylene trifluoromethylcarbonate.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116093267A (en) * | 2022-12-31 | 2023-05-09 | 安徽理士新能源发展有限公司 | Preparation method of negative electrode slurry, negative electrode plate and lithium battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116093267A (en) * | 2022-12-31 | 2023-05-09 | 安徽理士新能源发展有限公司 | Preparation method of negative electrode slurry, negative electrode plate and lithium battery |
| CN116093267B (en) * | 2022-12-31 | 2024-06-25 | 安徽理士新能源发展有限公司 | Preparation method of negative electrode slurry, negative electrode plate and lithium battery |
| WO2024139638A1 (en) * | 2022-12-31 | 2024-07-04 | 安徽理士新能源发展有限公司 | Preparation method for negative electrode slurry, negative electrode slurry, negative electrode sheet and lithium battery |
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