CN107492660B - Positive electrode slurry, positive plate and lithium ion battery - Google Patents
Positive electrode slurry, positive plate and lithium ion battery Download PDFInfo
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
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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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Abstract
本发明提供一种正极浆料、正极片及锂离子电池。所述正极浆料包括正极活性材料以及溶剂。所述正极浆料还包括正极添加剂，所述正极添加剂包括式1所示的聚苯基膦酸二苯砜酯。在式1中，n为1～30。当本发明的正极浆料应用在锂离子电池中后，在不影响锂离子电池的能量密度的前提下，能够大大提高锂离子电池的高温存储性能、高温循环性能和倍率性能。 The invention provides a positive electrode slurry, a positive electrode sheet and a lithium ion battery. The positive electrode slurry includes a positive electrode active material and a solvent. The positive electrode slurry further includes a positive electrode additive, and the positive electrode additive includes the polyphenylphosphonic acid diphenylsulfone ester shown in formula 1. In Formula 1, n is 1-30. When the positive electrode slurry of the present invention is applied in a lithium ion battery, the high temperature storage performance, high temperature cycle performance and rate performance of the lithium ion battery can be greatly improved without affecting the energy density of the lithium ion battery. 
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a positive electrode slurry, a positive plate and a lithium ion battery.
Background
With the increasingly wide application of electronic products such as smart phones, notebook computers and tablet computers, lithium ion batteries have the characteristics of high energy density, no memory effect, high working voltage and the like as the working power supply of the electronic products, and are gradually replacing the traditional Ni-Cd and MH-Ni batteries. However, with the expansion of market demand of electronic products and the development of power and energy storage devices, people have continuously increased requirements on lithium ion batteries, and it is urgent to develop lithium ion batteries having high energy density and satisfying rapid charging and discharging.
The methods for improving the rate capability of lithium ion batteries in the prior art are as follows. The first is to improve the rate capability and cycle performance of the lithium ion battery by optimizing the electrolyte composition. The second is to change the composition of the positive active material, for example, to improve rate capability by using a lithium iron phosphate/carbon composite positive active material; LiFePO is doped by selecting TiN phase4The rate capability is improved; the rate capability is improved by selecting the lithium manganate anode active material. But this method is applicable to only a single positive active material. The third is to make the lithium ion batteryThe particles of the positive and negative electrode active materials of (1) are nano-sized.
Although the rate performance of the lithium ion battery is improved to a certain extent by the methods, the cycle stability and the high-temperature storage performance of the lithium ion battery are reduced at the same time.
Disclosure of Invention
In view of the problems in the background art, an object of the present invention is to provide a positive electrode slurry, a positive electrode sheet, and a lithium ion battery, wherein the positive electrode slurry can greatly improve the high-temperature storage performance, the high-temperature cycle performance, and the rate capability of the lithium ion battery after being applied to the lithium ion battery without affecting the energy density of the lithium ion battery.
In order to achieve the above object, in one aspect of the present invention, there is provided a positive electrode slurry including a positive electrode active material and a solvent. The positive electrode slurry also comprises a positive electrode additive, and the positive electrode additive comprises polyphenyl phosphonic acid diphenyl sulfone ester shown in a formula 1. In formula 1, n is 1 to 30.
In another aspect of the present invention, the present invention provides a positive electrode sheet including a positive electrode current collector and a positive electrode membrane on the positive electrode current collector. The positive electrode membrane includes a positive electrode active material. The positive electrode diaphragm further includes: the positive electrode additive comprises polyphenyl phosphonic acid diphenyl sulfone ester shown in a formula 1. In formula 1, n is 1 to 30.
In still another aspect of the present invention, the present invention provides a lithium ion battery comprising the positive electrode sheet according to another aspect of the present invention.
Compared with the prior art, the invention has the beneficial effects that:
the positive electrode slurry contains the polyphenyl phosphonic acid diphenyl sulfone ester, and the high-temperature storage performance, the high-temperature cycle performance and the rate capability of the lithium ion battery can be greatly improved by applying the positive electrode slurry to the lithium ion battery on the premise of not influencing the energy density of the lithium ion battery.
The anode slurry is easy to prepare, good in repeatability, low in manufacturing cost and beneficial to large-scale industrial production.
Detailed Description
The positive electrode slurry, the positive electrode sheet and the lithium ion battery according to the present invention are described in detail below.
First, the cathode paste according to the first aspect of the invention is explained.
The positive electrode slurry according to the first aspect of the invention includes a positive electrode active material and a solvent. The positive electrode slurry also comprises a positive electrode additive, and the positive electrode additive comprises polyphenyl phosphonic acid diphenyl sulfone ester shown in a formula 1. In formula 1, n is 1 to 30.
In the positive electrode slurry according to the first aspect of the present invention, in the charging process of the polyphenyl phosphonic acid diphenyl sulfone ester, the sulfone ester functional group and the phenyl functional group are disconnected, so that a film can be coated on the surface of the positive electrode active material, the active site of the positive electrode active material is improved, and the reaction between the surface of the positive electrode active material and the electrolyte is inhibited, so that the high temperature storage performance, the high temperature cycle performance and the rate capability of the lithium ion battery can be improved without affecting the energy density of the lithium ion battery.
In the positive electrode slurry according to the first aspect of the present invention, n is preferably 20 to 25.
In the positive electrode slurry according to the first aspect of the invention, the weight of the positive electrode additive is 0.01% to 5% of the weight of the positive electrode active material. When the content of the positive electrode additive is too low, the performance improvement effect on the lithium ion battery is not obvious. When the content of the positive electrode additive is excessively high, the resistance of the electrode increases due to the non-conductive property of the positive electrode additive, resulting in deterioration of high-temperature cycle performance of the lithium ion battery. Preferably, the weight of the positive electrode additive is 0.05 to 0.5% of the weight of the positive electrode active material.
In the positive electrode slurry according to the first aspect of the invention, the specific kind of the positive electrode active material is not particularly limited and may be selected according to actual needs. Specifically, the positive active material is selected from one or more of transition metal oxides of lithium, transition metal oxides of lithium coated with inorganic compounds. The method of coating the surface of the lithium transition metal oxide with the inorganic compound is not particularly limited, and may be selected according to actual requirements, as long as the selected inorganic compound is coated on the surface of the lithium transition metal oxide.
In the positive electrode slurry according to the first aspect of the present invention, in the transition metal oxide of lithium coated with an inorganic compound, the weight of the inorganic compound is 0.005% to 5% of the weight of the transition metal oxide of lithium. Preferably, the weight of the inorganic compound is 0.05 to 4% of the weight of the transition metal oxide of lithium. More preferably, the weight of the inorganic compound is 0.05 to 3% of the weight of the transition metal oxide of lithium. Still more preferably, the weight of the inorganic compound is 0.05% to 2% of the weight of the transition metal oxide of lithium.
In the positive electrode slurry according to the first aspect of the present invention, the transition metal oxide of lithium is selected from LiCoO2、LiMn2O4、LiMnO2、Li2MnO4、LiFePO4、LiMn1-xMxO2、Li1+aMn1-xM’xO2、LiCo1-xAxO2、LiMn2- yB’yO4、Li2Mn1-xO4、LiFe1-xCxPO4One or more of them. Wherein, 0<a<0.2，0<x<1，0<y<2。
In the positive electrode slurry according to the first aspect of the invention, LiMn1-xMxO2、Li1+aMn1-xM’xO2To LiMnO of2And doping to obtain the doped material. The doping element M is not particularly limited, and may be selected according to actual requirements. Specifically, M is selected from one or more of Ni, Co, Al, Cr, Mg, Zr, Mo, V, Ti, B, F and Y. Preferably, M is selected from one or more of Co, Al, Cr, Mg, Zr, Ti and Y. Further preferably, M is selected from one or more of Al, Cr, Mg, Zr, Ti and Y. More preferably, M is one or more selected from Al, Cr, Mg, Ti and Y. The doping element M' is not particularly limited and may be selected according to practical requirements. Specifically, M' is selected from one or more of Ni, Co, Mn, Al, Cr, Mg, Zr, Mo, V, Ti, B, F and Y. Preferably, M' is selected from one or more of Co, Mn, Al, Cr, Mg, Zr, Ti and Y. Further preferably, M' is selected from one or more of Mn, Al, Cr, Mg, Zr, Ti and Y. More preferably, M' is one or more selected from Al, Cr, Mg, Ti and Y.
In the positive electrode slurry according to the first aspect of the invention, LiCo1-xAxO2To LiCoO2And doping to obtain the doped material. The doped element a is not particularly limited, and may be selected according to actual requirements. Specifically, A is selected from one or more of Ni, Al, Cr, Mg, Zr, Mo, V, Ti, B, F and Y. Preferably, A is selected from one or more of Co, Al, Cr, Mg, Zr, Ti and Y. Further preferably, A is selected from one or more of Al, Cr, Mg, Zr, Ti and Y. More preferably, A is selected from one or more of Al, Cr, Mg, Ti and Y.
In the positive electrode slurry according to the first aspect of the invention, LiMn2-yB’yO4To LiMn2O4And doping to obtain the doped material. The doped element B' is not particularly limited, and may be selected according to actual requirements. Specifically, B' is selected from one or more of Ni, Co, Al, Cr, Mg, Zr, Mo, V, Ti, B, F and Y. Preferably, B' is selected from one or more of Co, Al, Cr, Mg, Zr, Ti and Y. Further preferably, B' is selected from Al, Cr, Mg, Zr, TiAnd one or more of Y. More preferably, B' is one or more selected from Al, Cr, Mg, Ti and Y.
In the positive electrode slurry according to the first aspect of the invention, LiFe1-xCxPO4For LiFePO4And doping to obtain the doped material. The doping element C is not particularly limited, and may be selected according to actual requirements. Specifically, C is selected from one or more of Ni, Co, Mn, Al, Cr, Mg, Zr, Mo, V, Ti, B, F and Y. Preferably, C is selected from one or more of Co, Mn, Al, Cr, Mg, Zr, Ti and Y. Further preferably, C is selected from one or more of Mn, Al, Cr, Mg, Zr, Ti and Y. More preferably, C is selected from one or more of Al, Cr, Mg, Ti and Y.
In the positive electrode slurry according to the first aspect of the present invention, the method of doping is not particularly limited, and may be selected according to actual needs as long as the selected element is doped into the positive electrode active material. In particular, bulk doping is selected to dope the selected elements into the positive active material.
In the positive electrode slurry according to the first aspect of the present invention, preferably, the positive electrode active material is selected from doped positive electrode active materials, i.e., selected from LiMn1-xMxO2、Li1+aMn1-xM’xO2、LiCo1-xAxO2、LiMn2-yB’yO4、Li2Mn1- xO4、LiFe1-xCxPO4One or more of them. The doped positive active material can further improve the rate capability of the lithium ion battery, and does not influence the high-temperature storage performance and the high-temperature cycle performance of the lithium ion battery. Still more preferably, the positive electrode active material is selected from positive electrode active materials obtained by coating inorganic compounds on the surface of the doped positive electrode active material, namely selected from LiMn respectively coated with inorganic compounds1-xMxO2、Li1+aMn1-xM’xO2、LiCo1-xAxO2、LiMn2-yB’yO4、Li2Mn1-xO4、LiFe1-xCxPO4One or more of them.
In the positive electrode slurry according to the first aspect of the present invention, the doping elements (M, M ', A, B', C) are present in a weight ratio to the base material (i.e., LiCoO, which is a positive electrode active material before being undoped)2、LiMn2O4、LiMnO2、Li2MnO4、LiFePO4) 0.01 to 10% by weight of (A). Preferably, the weight of the doping element is 0.05-5% of the weight of the base material. More preferably, the weight of the doping element is 0.05 to 3% of the weight of the base material. More preferably, the weight of the doping element is 0.05-1.5% of the weight of the base material.
In the positive electrode slurry according to the first aspect of the invention, the inorganic compound is selected from Al2O3、AlF3、AlPO4、Li3PO4、Li4P2O7、ZrO2、MgO、TiO2、Y2O3、LiAlO2、LiNiPO4One or more of them. Preferably, the inorganic compound is selected from Al2O3、AlPO4、Li3PO4、Li4P2O7、ZrO2、MgO、TiO2、Y2O3、LiNiPO4One or more of them. Further preferably, the inorganic compound is selected from Al2O3、ZrO2、MgO、TiO2、Y2O3One or more of them. Even more preferably, the inorganic compound is selected from Al2O3、MgO、TiO2One or more of them.
In the positive electrode slurry according to the first aspect of the invention, the positive electrode slurry further includes a conductive agent.
In the positive electrode slurry according to the first aspect of the present invention, the kind of the conductive agent is not particularly limited, and may be selected according to actual needs. Specifically, the conductive agent is selected from one or more of conductive carbon black, superconducting carbon black, conductive graphite, acetylene black and carbon nanotubes. Preferably, the conductive agent is selected from one or more of conductive carbon black, conductive graphite and acetylene black. Further preferably, the conductive agent is selected from one or more of conductive carbon black and acetylene black. Still more preferably, the conductive agent is selected from conductive carbon black. The conductive carbon black may be Super-P.
In the positive electrode slurry according to the first aspect of the present invention, the weight of the conductive agent is 0.005 to 5% of the weight of the positive electrode active material. Preferably, the weight of the conductive agent is 0.05-4% of the weight of the positive electrode active material. Further preferably, the weight of the conductive agent is 0.05-3% of the weight of the positive electrode active material. Still more preferably, the weight of the conductive agent is 0.05 to 2% of the weight of the positive electrode active material.
In the positive electrode slurry according to the first aspect of the invention, the positive electrode slurry further includes a binder.
In the positive electrode slurry according to the first aspect of the invention, the specific kind of the binder is not particularly limited as long as it can function as a binder. Specifically, the binder is selected from one or more of polyvinyl alcohol, polyurethane, polyacrylate, polyvinylidene fluoride (PVDF), butyl rubber, epoxy resin, vinyl acetate resin and chlorinated rubber. Preferably, the binder is selected from one or more of polyurethane, epoxy resin, polyvinylidene fluoride and polyacrylate.
In the positive electrode slurry according to the first aspect of the invention, the weight of the binder is 0.005% to 5% of the weight of the positive electrode active material. Preferably, the weight of the binder is 0.05 to 4% of the weight of the positive electrode active material. Further preferably, the weight of the binder is 0.05% to 3% of the weight of the positive electrode active material. Still more preferably, the weight of the binder is 0.05% to 2% of the weight of the positive electrode active material.
In the positive electrode slurry according to the first aspect of the present invention, the specific kind of the solvent is not particularly limited, and may be selected according to actual needs. Preferably, the solvent is an organic solvent. The organic solvent is one or more selected from tetrahydrofuran, pyridine, N-methyl pyrrolidone and pyrrole. Preferably, the organic solvent is one or more selected from tetrahydrofuran and N-methyl pyrrolidone. Further preferably, the organic solvent is selected from N-methylpyrrolidone.
In the positive electrode slurry according to the first aspect of the invention, the weight of the solvent is 0.01 to 50 times the weight of the positive electrode active material. Preferably, the weight of the solvent is 0.1 to 35 times of the weight of the positive electrode active material. Further preferably, the weight of the solvent is 1 to 10 times of the weight of the positive electrode active material. Still more preferably, the weight of the solvent is 1.5 to 6 times of the weight of the positive electrode active material.
In the positive electrode slurry according to the first aspect of the present invention, the method for preparing the positive electrode slurry is not particularly limited, and a conventional method may be used. For example, a positive electrode active material, a positive electrode additive, a conductive agent, and a binder are added to a solvent and uniformly mixed to obtain a positive electrode slurry.
Next, the positive electrode sheet according to the second aspect of the invention is explained.
The positive electrode sheet according to the second aspect of the present invention includes a positive electrode current collector and a positive electrode membrane sheet on the positive electrode current collector. The positive electrode membrane includes the positive electrode active material according to the first aspect of the invention and a positive electrode additive.
In the positive electrode sheet according to the second aspect of the present invention, the positive electrode sheet may be formed from the positive electrode slurry according to the first aspect of the present invention at least after drying. Wherein the drying is used to remove the solvent from the positive electrode slurry. As for the amount of the solvent remaining in the positive electrode sheet formed after the positive electrode slurry is dried, it can be determined depending on the requirements of the specific production situation. The term "at least dried" refers to a step of removing the solvent in the positive electrode slurry to form a positive electrode membrane, and of course, other steps such as cold pressing, slitting, etc. are provided according to actual production conditions, and the invention is not limited to this.
In the positive electrode sheet according to the second aspect of the present invention, the positive electrode sheet may further include the conductive agent according to the first aspect of the present invention.
In the positive electrode sheet according to the second aspect of the invention, the positive electrode sheet may further include a binder according to the first aspect of the invention.
In the positive electrode sheet according to the second aspect of the present invention, the positive electrode current collector is an aluminum foil.
In the positive electrode sheet according to the second aspect of the invention, the thickness of the positive electrode current collector is 5 to 30 μm. Preferably, the thickness of the positive electrode current collector is 12 micrometers.
The lithium ion battery according to the third aspect of the invention is explained again.
A lithium ion battery according to a third aspect of the invention includes the positive electrode sheet according to the second aspect of the invention.
The lithium ion battery according to the third invention further includes a negative electrode sheet, an electrolyte, and a separator.
In the lithium ion battery according to the third aspect of the present invention, the specific types of the negative electrode sheet, the electrolyte and the separator are not particularly limited, and may be selected according to actual needs.
The present application is further illustrated below with reference to 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.
In the following examples, materials, reagents and instruments used were commercially available, unless otherwise specified.
For convenience of explanation, the positive electrode active material and the positive electrode additive used in the following examples are abbreviated as follows:
positive electrode active material 1: in LiCoO2Medium doped occupied LiCoO20.1% by weight of Al and LiCoO20.1% by weight of Mg, and then coating Al on the surface of the doped material in an amount of 0.1% by weight of the doped material2O3And TiO accounting for 0.1 percent of the weight of the doping material2。
Positive electrode active material 2: LiFePO4。
Positive electrode active material 3: LiCo0.8Ni0.2O2。
Positive electrode additive 1: the degree of polymerization n is 10.
Positive electrode additive 2: the degree of polymerization n is 15.
Positive electrode additive 3: the degree of polymerization n is 20.
Positive electrode additive 4: the degree of polymerization n is 25.
(1) Preparation of positive plate
Mixing a positive electrode active material, a positive electrode additive, a binder and a conductive agent, adding a solvent N-methylpyrrolidone (NMP), and uniformly stirring under the action of a vacuum stirrer to obtain positive electrode slurry; uniformly coating the positive electrode slurry on an aluminum foil with the thickness of 12 mu m; and (3) airing the aluminum foil at room temperature, transferring the aluminum foil to a 90 ℃ oven for drying for 1h, and then carrying out cold pressing and slitting to obtain the positive plate, wherein the positive plate slurry finally forms a positive membrane. The kinds and contents of the positive electrode active material, the positive electrode additive, the binder, and the conductive agent are shown in table 1. The content is the weight percentage of all substances in the total weight of the positive active material, the positive additive, the binder and the conductive agent.
(2) Preparation of negative plate
Mixing graphite serving as a negative electrode active material, sodium carboxymethyl cellulose (CMC) serving as a thickening agent and styrene butadiene rubber serving as a binder according to a weight ratio of 98:1:1, adding deionized water serving as a solvent, and uniformly stirring under the action of a vacuum stirrer to obtain negative electrode slurry; uniformly coating the negative electrode slurry on a copper foil with the thickness of 8 mu m; and (3) airing the copper foil at room temperature, transferring the copper foil to a 120 ℃ oven for drying for 1h, and then carrying out cold pressing and slitting to obtain a negative plate, wherein the negative plate slurry finally forms a negative membrane.
(3) Preparation of electrolyte
At water content<In a 10ppm argon atmosphere glove box, a fully dried lithium salt LiPF6Dissolving in organic solvent, and mixing to obtain electrolyte. Wherein, LiPF6Is 1M. Wherein the organic solvent is ethylene carbonate, propylene carbonate and propyl propionate which are 1:1:1 (solid)Volume ratio).
(4) Preparation of the separator
A 14 micron thick polypropylene separator (available from Celgard) was selected.
(5) Preparation of lithium ion battery
Stacking the positive plate, the isolating film and the negative plate in sequence to enable the isolating film to be positioned between the positive plate and the negative plate to play an isolating role, and then winding to obtain a battery cell; and placing the battery cell in an aluminum-plastic film for baking, injecting the prepared electrolyte into the dried battery cell for sealing and standing, and then carrying out procedures such as formation, aging and the like on the battery cell to obtain the lithium ion battery.
Next, performance tests of the lithium ion battery are explained. Wherein, each group tests 15 lithium ion batteries, and the average value is taken.
(1) Rate capability test of lithium ion battery
At 25 ℃, the lithium ion battery is charged to 4.35V by a constant current of 1C (nominal capacity), then charged by a constant voltage of 4.35V until the current is less than or equal to 0.05C, and after being placed for 5min, the lithium ion battery is discharged by a constant current of 0.2C until the cut-off voltage is 3V, and at this time, the actual discharge capacity is recorded as D0. Then charging to 4.35V by a constant current of 1C, then charging to a current of less than or equal to 0.05C by a constant voltage of 4.35V, finally discharging to a cut-off voltage of 3V by 2C, and recording the actual discharge capacity at the moment as D1. The rate capability of the lithium ion battery is [ (D1-D0)/D0] multiplied by 100%.
(2) High temperature storage performance testing of lithium ion batteries
Charging the lithium ion battery to 4.35V at a constant current of 0.5C at 60 ℃, then charging the lithium ion battery at a constant voltage until the current is 0.05C, and testing the thickness of the lithium ion battery and recording the thickness as h0(ii) a Then the lithium ion battery is placed into a constant temperature box with the temperature of 60 ℃, stored for 30 days, taken out on the 30 th day, tested and recorded as h for the thickness of the lithium ion battery at the moment1. The lithium ion battery has a thickness expansion rate (h) after 30 days of storage at 60 DEG C1-h0)/h0]×100％。
(3) High temperature cycle performance testing of lithium ion batteries
At 45 ℃, the lithium ion battery is charged to 4.35V at a constant current of 1C, then charged at a constant voltage until the current is 0.05C, and then discharged to 3.0V at a constant current of 1C, at this time, the first cycle, and 300 cycles of charge/discharge are performed according to the above conditions. The capacity retention ratio after the lithium ion battery was cycled 300 times at 45 ═ 100% (discharge capacity of 300 cycles/discharge capacity of the first cycle).
Table 2 results of performance test of lithium ion batteries of examples 1 to 9 and comparative examples 1 to 3
From the test results in table 2, it can be seen that the rate performance, high-temperature cycle performance and high-temperature storage performance of the lithium ion battery added with the positive electrode additive of the polyphenyl diphenyl sulfone phosphonate ester are obviously improved compared with those of the comparative examples 1 to 3.
Claims (11)
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