CN106684320B - A kind of positive pole piece, its preparation method and secondary battery - Google Patents
A kind of positive pole piece, its preparation method and secondary battery Download PDFInfo
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- H01M4/00—Electrodes
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Abstract
本申请涉及一种正极极片，包括正极集流体和涂覆于正极集流体上的正极膜片，正极膜片中含有正极活性材料、导电剂和粘结剂，正极膜片中还含有导电添加剂，导电添加剂为负温度系数半导体陶瓷材料。通过使用该导电添加剂能够解决当前二次电池在低温充电过程中容易析锂，从而导致电池容量衰减快，安全风险高的问题，且不影响电池在常温及高温下的使用。The present application relates to a positive electrode sheet, comprising a positive electrode current collector and a positive electrode film coated on the positive electrode current collector, the positive electrode film contains a positive electrode active material, a conductive agent and a binder, and the positive electrode film also contains a conductive additive , the conductive additive is a negative temperature coefficient semiconductor ceramic material. The use of the conductive additive can solve the problem that the current secondary battery is prone to lithium precipitation during low-temperature charging, resulting in rapid battery capacity decay and high safety risk, and does not affect the use of the battery at room temperature and high temperature.
Description
Technical Field
The application relates to the technical field of secondary batteries, in particular to a positive pole piece, a preparation method thereof and a secondary battery using the positive pole piece.
Background branch operation
In recent years, lithium ion batteries have been rapidly developed and the demand for such batteries has been increasing. Lithium ion batteries generally need to meet the following characteristics: (1) the hybrid electric vehicle has high energy and high power density, and has higher power requirement compared with an energy storage battery; (2) the working temperature range is wide, and the environmental suitability is strong; (3) long cycle life and service life; (4) outstanding safety and reliability.
Lithium ion batteries exhibit good performance at normal temperatures, while performance at low temperatures is significantly degraded. Low temperature to lithium ion batteryThe influence of energy mainly relates to the following aspects: (1) reducing the conductivity of the electrolyte and the SEI film; (2) limiting the diffusion of lithium ions in the graphite anode; (3) anodic polarization related to the first two factors; (4) increasing the resistance to charge transfer between the electrolyte/electrode interface. The negative electrode material used by the existing lithium ion battery is mainly graphite negative electrode material, and the lithium intercalation potential of the graphite material is relative to Li+the/Li is only 0.1-0.2V, the resistance of lithium ion and electron migration in the electrode material at low temperature is large, the resistance of the electrode is large, the polarization potential is large, the lithium intercalation potential of the graphite material is reduced, the lithium precipitation of the negative electrode is easily caused, and the process is irreversible. If the charging is repeated at low temperature, the capacity of the lithium ion battery can be rapidly reduced, and the service life of the lithium ion battery is shortened. Meanwhile, metal lithium may be precipitated on the surface of the carbon electrode to form lithium dendrite, and the dendrite further grows to pierce through the diaphragm, so that the anode and the cathode are connected, short circuit is caused, damage is caused to the battery, and the safety of the battery is reduced. Particularly, the safety performance of the lithium ion battery is greatly damaged when the lithium ion battery is extruded and impacted by the outside.
In view of the above, it is desirable to provide a lithium ion battery having good resistance to lithium deposition at low temperatures.
Disclosure of Invention
The primary purpose of the present application is to provide a positive electrode sheet.
The second invention of the application aims to provide a preparation method of the positive pole piece.
A third aspect of the present invention is to provide a secondary battery using the positive electrode sheet.
In order to accomplish the purpose of the application, the technical scheme is as follows:
the application relates to a positive pole piece, including the anodal mass flow body and coat in anodal diaphragm on the anodal mass flow body, contain anodal active material, conductive agent, binder and conductive additive in the anodal diaphragm, conductive additive is negative temperature coefficient semiconductor ceramic material.
Preferably, the conductive additive is La (Mn)xTiy)O3Wherein 0.6 is less than or equal tox≤0.7，0.3≤y≤0.4。
Preferably, the particle size of the conductive additive is 0.01 to 15 μm.
Preferably, the mass percentage of the conductive additive in the positive electrode membrane is 0.01-5%, preferably 0.05-0.5%.
Preferably, the mass ratio of the positive electrode active material, the conductive agent and the adhesive in the positive electrode membrane is (88-98): 1-7): 1-5.
Preferably, the conductive agent is selected from at least one of a zero-dimensional carbon material, a one-dimensional carbon material, and a two-dimensional carbon material.
Preferably, the zero-dimensional carbon material is at least one of conductive carbon black and acetylene black; the one-dimensional carbon material is selected from at least one of carbon fiber and carbon nano tube; the two-dimensional carbon material is selected from at least one of graphite, graphene and carbon nanoribbons.
Preferably, the binder is an aqueous binder or an oily binder, the aqueous binder is selected from at least one of styrene-butadiene rubber, aqueous acrylic resin and carboxymethyl cellulose, and the oily binder is selected from at least one of polyvinylidene fluoride, ethylene-vinyl acetate copolymer and polyvinyl alcohol.
The application also relates to a preparation method of the secondary battery positive pole piece, which is characterized in that positive pole slurry comprising the positive pole active material, a conductive agent, a binder and a conductive additive is coated on the surface of a positive pole current collector, and a positive pole diaphragm is formed after drying, so that the positive pole piece is obtained.
The application also relates to a secondary battery, which uses the positive pole piece.
The technical scheme of the application has at least the following beneficial effects:
the application provides a positive pole piece, its conductive additive is the conductive additive of negative temperature coefficient semiconductor, can solve present secondary battery and analyse lithium easily in low temperature charging process to lead to the battery capacity decay fast, the problem that the safety risk is high, and does not influence the use of battery under normal atmospheric temperature and high temperature, guarantee the validity of electrically conductive network, the life of extension electric core.
Detailed Description
The present application is further illustrated with reference to specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present application.
The application relates to a positive pole piece, including the anodal mass flow body and coat in anodal diaphragm on the anodal mass flow body contains anodal active material, conductive agent, binder and conductive additive in the anodal diaphragm, and conductive additive is negative temperature coefficient semiconductor ceramic material. In the prior art, ceramic materials are mostly used for coating the separator to improve the safety of the separator and the lithium ion transfer rate, and the ceramic materials are used for a current collector and are rarely reported as conductive additives. The negative temperature coefficient semiconductor ceramic material is used in the positive diaphragm, so that the impedance and polarization of the positive electrode at low temperature can be increased, the charging platform of negative electrode graphite is improved, the secondary battery, particularly the lithium ion battery, is easy to separate lithium in the low-temperature charging process, and the problems of fast battery capacity attenuation, high safety risk and the like are caused.
As an improvement of the positive pole piece of the application, the conductive additive is La (Mn)xTiy)O3Wherein x is more than or equal to 0.6 and less than or equal to 0.7, and y is more than or equal to 0.3 and less than or equal to 0.4. La (Mn)xTiy)O3The material is an improved negative temperature coefficient semiconductor ceramic material, has larger impedance at low temperature, and has excellent conductivity and stability at normal temperature and high temperature. In the charging process at low temperature, the resistance in the transition coating is rapidly increased, namely, the resistance between the positive active material and the current collector is increased, and the polarization potential of the positive electrode is further increased, so that the charging voltage rapidly reaches the cut-off voltage, and the lithium is not separated out on the surface of the negative electrode material at low temperature. When the temperature returns to normal, the resistance of the transition layer is reduced, a good electronic path is restored between the positive active material and the current collector, and the battery starts to be charged normally.
As an improvement of the positive pole piece, the particle size of the conductive additive is 0.01-15 μm. When the particle size is too small and is less than 0.01 μm, on one hand, the manufacturing cost is increased, and on the other hand, the processability of the positive electrode slurry is affected; when the particle diameter is larger than 15 μm, the positive electrode slurry is likely to form particles upon coating, and may pierce through a separator (the thickness of a separator is usually 7 to 16 μm), resulting in a risk of internal short circuit of the battery.
As an improvement of the positive pole piece, the mass percentage of the conductive additive in the positive pole membrane is 0.01-5%, preferably 0.05-0.5%. The mass content of the conductive additive is too low, so that the resistance in the transition layer under low-temperature charging is hardly influenced, and the improvement of lithium separation is not obvious. The mass content of the conductive additive is too high, and the resistance between the current collector and the positive electrode active material is too large, so that the transmission of lithium ions between the positive electrode and the negative electrode is influenced.
As an improvement of the positive pole piece, the mass ratio of the positive active material, the conductive agent and the adhesive in the positive membrane is (88-98) to (1-7) to (1-5).
As an improvement of the positive pole piece, the conductive agent is at least one selected from zero-dimensional carbon materials, one-dimensional carbon materials and two-dimensional carbon materials; preferably, the zero-dimensional carbon material is at least one of conductive carbon black and acetylene black; the one-dimensional carbon material is selected from at least one of carbon fiber and carbon nano tube; the two-dimensional carbon material is selected from at least one of graphite, graphene and carbon nanoribbons. Commonly used conductive agents include Ketjen black (ultra fine conductive carbon black, particle size 30-40nm), SP (Super P, small particle conductive carbon black, particle size 30-40 μm), S-O (ultra fine graphite powder, particle size 3-4 μm), KS-6 (large particle graphite powder, particle size 6.5 μm), acetylene black, VGCF (vapor grown carbon fiber, particle size 3-20 μm).
As an improvement of the positive pole piece, the binder is a water-based binder or an oil-based binder, the water-based binder is at least one selected from styrene-butadiene rubber, water-based acrylic resin and carboxymethyl cellulose, and the oil-based binder is at least one selected from polyvinylidene fluoride, ethylene-vinyl acetate copolymer and polyvinyl alcohol (PVA).
The application also relates to a preparation method of the conductive additive, which comprises the following steps:
1) mixing a lanthanum source compound and a manganese source compound, and performing ball milling to obtain a first mixture;
2) adding a titanium source compound into the first mixture, and performing ball milling to obtain a second mixture;
3) and sintering the second mixture to obtain the conductive additive.
Further, the lanthanum source compound in step 1) may be La2O3The manganese source compound may be Mn2O3Or both the lanthanum source compound and the manganese source compound are LaMnO3(ii) a The titanium source compound in the step 2) is Ti2O3. In the application, the lanthanum source compound, the manganese source compound and the titanium source compound are all selected from oxides, so that the introduction of other types of ions caused by the use of salts of the elements can be avoided.
Preferably, the molar ratio of the lanthanum, manganese and titanium elements in the second mixture is 1: 0.6-0.7: 0.3-0.4.
Preferably, the sintering temperature in the step 3) is 1000-1500 ℃, and the sintering time is 4-8 h.
In the application, the positive electrode slurry comprising the positive electrode active material, the conductive agent, the binder and the conductive additive is coated on the surface of the positive electrode current collector, and a positive electrode diaphragm is formed after drying, so that the positive electrode plate of the secondary battery is obtained.
The application also relates to a secondary battery which uses the positive pole piece. Specifically, the secondary battery contains a positive electrode plate, a negative electrode plate, a separator and an electrolyte. The positive plate comprises a positive current collector and a positive membrane coated on the positive current collector; the negative plate comprises a negative current collector and a negative diaphragm coated on the negative current collector; the electrolyte comprises lithium salt and organic solvent; the isolation film is positioned between the adjacent positive and negative pole pieces.
As an improvement of the secondary battery of the present application, the positive electrode active material is selected from lithium cobaltate, lithium manganate, lithium nickel cobalt manganate Li (Ni)xMnyCoz)O2(0<x,y,z<1; x + y + z ═ 1); the negative active material is selected from one or more of natural graphite, artificial graphite, soft carbon, hard carbon, lithium titanate and silicon.
As an improvement of the secondary battery of the present application,the lithium salt is selected from lithium hexafluorophosphate LiPF6Lithium tetrafluoroborate (LiBF)4Lithium bis (oxalato) borate LiB (C)2O4)2(abbreviated as LiBOB) and lithium difluorooxalato borate LiBF2(C2O4) (abbreviated as LiDFOB) and lithium hexafluoroarsenate (LiAsF)6) Lithium perchlorate (LiClO)4) Lithium tris (perfluoroethyl) trifluorophosphate LiFAP, lithium trifluoromethanesulfonate LiCF3SO3Bis (trifluoromethylsulfonic acid) methyllithium Li (FSO)2)2Lithium N, bis (trifluoromethylsulfonate) imido LiN (CF)3SO2)2Lithium bis (perfluoroethylsulfonate) imide Li (C)2F5SO2)2N、Li(C4F9SO2)2N、Li(SO2(CF2)3SO2)2At least one of N, the lithium salt is preferably LiPF6、LiBF4、Li(FSO2)2And N.
As an improvement of the secondary battery, the organic solvent is selected from carbonate, sulfate, sulfone, nitrile compound and the like, and the carbonate is selected from cyclic carbonate and chain carbonate; the sulfate is selected from cyclic sulfate, chain sulfate, etc. The organic solvent which can be specifically selected from the following is not limited thereto: at least one of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, dipropyl carbonate, ethyl methyl carbonate, methyl formate, ethyl propionate, propyl propionate, methyl butyrate, ethyl acetate, ethylene sulfite, fluoroethylene carbonate, propane sultone, N-methylpyrrolidone, N-methylformamide, N-methylacetamide, acetonitrile, acrylonitrile, gamma-butyrolactone, methyl sulfide, cyclohexylbenzene, and biphenyl.
Example 1
Preparing a positive plate:
dissolving polyvinylidene fluoride (PVDF) as a binder in N-methylpyrrolidone (NMP) as a solvent, fully stirring, and then adding a positive active material, a conductive agent Super P and a conductive additive. Wherein the positive active substance is nickel-cobalt-manganese ternary material LiNi0.5Co0.2Mn0.3O2Particle diameter D of conductive additive50Is 10 μm. And finally, vacuumizing to remove bubbles. Filtering the mixture by using a 150-mesh stainless steel screen to obtain the required anode slurry. And uniformly coating the obtained positive electrode slurry on a positive electrode current collector aluminum foil, drying at 85 ℃, and performing cold pressing and sheet cutting after drying to obtain the positive electrode piece. The sample numbers and the raw material ratios of the positive electrode pieces are shown in table 1.
TABLE 1
Preparing a negative plate:
dissolving Styrene Butadiene Rubber (SBR) serving as a binder in water to obtain an SBR aqueous solution, adding artificial graphite, Super P and carboxymethyl cellulose sodium (CMC) serving as a thickener into the SBR aqueous solution, uniformly stirring, coating the mixture on a copper foil with the thickness of 8 mu m, drying at 110 ℃, and performing cold pressing and cutting to obtain a negative pole piece, wherein the weight ratio of the artificial graphite to the Super P to CMC2200 to the SBR is 96:1:1: 2;
the isolation film is a polypropylene (PP)/Polyethylene (PE)/polypropylene (PP) three-layer composite porous film with the thickness of 12 mu m;
preparing an electrolyte:
uniformly mixing equal volume of Ethylene Carbonate (EC), Ethyl Methyl Carbonate (EMC) and diethyl carbonate (DEC) to obtain a mixed solvent, and adding lithium hexafluorophosphate (LiPF)6) Wherein LiPF6The concentration of (2) is 1 mol/L.
And (3) forming a battery core by winding or laminating the positive plate, the negative plate and the isolating film, then placing the battery core into a packaging bag, injecting electrolyte, and then forming, packaging, capacity and the like to assemble the battery. The cell obtained with P1 as the positive electrode tab was designated C1, and the cell obtained with P2 as the positive electrode tab was designated C2. And the same process is repeated to obtain cell samples C1-C11.
Comparative example 1
The positive electrode diaphragm does not contain a conductive additive, the obtained positive electrode piece is marked as P1#, other steps are the same as those of the embodiment 1, and the obtained battery is marked as C1 #.
Comparative example 2
The conductive additive is LaMnO3The obtained positive pole piece is marked as P2#, the other steps are the same as the example 1, and the obtained battery is marked as C2 #.
Comparative example 3
And adding a conductive additive into the negative electrode diaphragm, and performing the same steps as in example 1 to obtain a battery marked as C3 #.
Test example
The following tests were carried out on the batteries obtained in example 1, and comparative examples 1 to 3:
1. the lithium deposition condition of the battery after 10 charge-discharge cycles at-5 ℃ is tested: the charging process comprises the steps of firstly carrying out constant current charging to 4.20V at a charging rate of 1C, and then carrying out constant voltage charging until the current is reduced to 0.05C; the discharge process is that the constant current is discharged to 2.8V at the discharge rate of 1C; and finally, fully charging the battery.
2. The lithium deposition condition of the battery after 10 charge-discharge cycles at-15 ℃ is tested: the charging process comprises the steps of firstly carrying out constant current charging to 4.20V at a charging rate of 0.5C, and then carrying out constant voltage charging until the current is reduced to 0.05C; the discharge process is that the constant current is discharged to 2.8V at the discharge rate of 1C; and finally, fully charging the battery.
3. The lithium deposition condition of the battery after 10 charge-discharge cycles at-25 ℃ is tested: the charging process comprises the steps of firstly carrying out constant current charging to 4.20V at a charging rate of 0.3C, and then carrying out constant voltage charging until the current is reduced to 0.05C; the discharge process is that the constant current is discharged to 2.8V at the discharge rate of 1C; and finally, fully charging the battery.
And (3) disassembling the battery, checking the lithium precipitation condition of the negative pole piece, and specifically showing the result in table 2.
TABLE 2
And (3) carrying out cycle performance tests on the batteries C1-C11 and C1-C3 respectively:
charging the lithium ion battery to 3.7V at a multiplying power of 0.3C, then charging the lithium ion battery to 4.2V at a constant current at a multiplying power of 0.5C, then charging the lithium ion battery at a constant voltage until the current is 0.05C, finally discharging the lithium ion battery to 2.8V at a constant current of 0.5C, and detecting to obtain the first efficiency. In addition, the lithium ion battery was constant-current charged to 4.2V at a rate of 1C, then constant-voltage charged to a current of 0.05C, and then constant-current discharged to 2.8V at a current of 0.5C, and under such charge/discharge cycle conditions, the capacity retention rates after the lithium ion battery was cycled 100 times, 500 times, 1000 times, and 1500 times, respectively, were examined at 45 ℃.
Wherein the first efficiency is (first discharge capacity/first charge capacity) × 100%, and the capacity retention rate after cycles is (discharge capacity after corresponding cycles/first discharge capacity) × 100%.
TABLE 3
Comparing the pole pieces P1-P7 and P10-P11 with other examples and comparative examples, it can be seen that when the dosage of the conductive additive in the positive pole membrane meets the mass percentage content range of 0.1-5%, the lithium precipitation condition of the battery does not occur. However, when the amount of the conductive additive is more than 5%, the cycle performance of the battery is affected to some extent.
In comparison with the electrode sheet P8, when the content of the conductive additive is too small and is 0.01%, lithium precipitation occurs when the temperature is reduced to-15 ℃ and-25 ℃, but the lithium precipitation performance is still improved to a certain extent compared with the comparative example 1 without the conductive additive. In comparison with the electrode sheet P9, when the content of the conductive additive is above 5%, although no lithium is separated from the battery cell, the amount of the cathode active material is reduced, and it is theoretically inferred that the energy density of the battery cell is also reduced, and the cycle performance of the battery is also greatly reduced in the actual test. Therefore, in order to ensure that the battery cell does not precipitate lithium at low temperature and has higher energy density, the weight content of the conductive additive needs to be controlled within the range of 0.01-5%, preferably 0.05-0.5%.
In contrast, comparative example 1, which did not use a conductive additive, slightly extracted lithium at-5 deg.C, -15 deg.C and-25 deg.C, and severely extracted lithium. The test results of comparative example 2 using other ceramic materials were the same as in comparative example 1, indicating that the conventional ceramic materials did not improve the lithium-extracting performance of the battery. And the conductive additive is applied to the negative electrode in the comparative example 3, and the serious lithium precipitation occurs at the temperature of minus 5 ℃, because the conductive additive has larger impedance at low temperature, and the conductive additive is applied to the negative electrode, so that the conductive capability of a negative electrode piece is reduced, the polarization potential of the negative electrode is increased, and the lithium precipitation potential is more easily reached in the charging process, so the low-temperature lithium precipitation phenomenon is serious.
Therefore, the lithium ion battery with better lithium separation resistance can be obtained, particularly, the lithium separation of the battery cell is avoided in the low-temperature charging process, and the safety performance of the battery in the service cycle is met.
Although the present application has been described with reference to preferred embodiments, it is not intended to limit the scope of the claims, and many possible variations and modifications may be made by one skilled in the art without departing from the spirit of the application.
Claims (11)
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| CN110165150A (en) * | 2018-01-09 | 2019-08-23 | 江西理工大学 | A kind of high capacity nickel-base anode material cell and its measurement method for internal resistance of discharging |
| TWI668902B (en) * | 2018-04-03 | 2019-08-11 | 臺灣塑膠工業股份有限公司 | Electrode and electrochemical energy storage device |
| CN114094051A (en) * | 2021-11-02 | 2022-02-25 | 珠海冠宇动力电池有限公司 | A positive electrode material and a lithium battery comprising the material |
| CN115411220A (en) * | 2022-09-13 | 2022-11-29 | 珠海冠宇电池股份有限公司 | Positive plates, cells and batteries |
| CN115832198B (en) * | 2022-11-30 | 2024-09-27 | 宁德时代新能源科技股份有限公司 | Electrode piece, electrode assembly, secondary battery and electrical device |
| CN116705987B (en) * | 2023-08-04 | 2024-01-26 | 深圳市德兰明海新能源股份有限公司 | Negative plate, electrochemical device and preparation method of electrochemical device |
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| CN202293491U (en) * | 2011-10-24 | 2012-07-04 | 杨桦 | Composite film for current collector of lithium ion battery |
| CN204577500U (en) * | 2015-04-17 | 2015-08-19 | 宁德时代新能源科技有限公司 | Barrier film, battery core and secondary cell |
| CN104868158A (en) * | 2015-05-06 | 2015-08-26 | 宁德新能源科技有限公司 | Lithium ion battery |
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