CN109841832B - Positive plate and electrochemical cell - Google Patents
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Abstract
The application provides a positive plate and an electrochemical cell. The positive plate comprises a positive current collector and a positive diaphragm, wherein the positive diaphragm is arranged on the positive current collector and comprises a positive active material, a conductive agent and a binder. The positive active material comprises a Prussian blue material, and the molecular formula of the Prussian blue material is AxMz[M′(CN)6]yWherein, A is one or more of alkali metal ions and alkaline earth metal ions, M is transition metal, M' is transition metal, x is more than 0 and less than or equal to 2, y is more than 0 and less than or equal to 1, z is more than 0 and less than or equal to 1, the particle size D50 of the Prussian blue material is 50 nm-10 mu M, and the porosity of the anode membrane is 10-50%. The positive plate can ensure that the electrochemical cell has better cycle performance and higher volume energy density, and is suitable for large-scale production.
Description
Technical Field
The application relates to the field of batteries, in particular to a positive plate and an electrochemical battery.
Background
Prussian Blue Analogue (PBA) materials have the advantages of high specific capacity, high voltage platform, low cost and the like, and are positive electrode materials which are widely concerned in recent years. In the preparation process of the prussian blue material, due to the high ion reaction speed, the particle size obtained is usually small (generally nano-scale or micron-scale), so that the particles are difficult to compact, which is not only unfavorable for establishing a conductive network between the particles, but also unfavorable for the overall design of the product because the volume energy density of the battery is reduced, and therefore, how to consider the volume energy density and the performance of the battery is one of the problems to be considered in the practical application of the prussian blue material.
Disclosure of Invention
In view of the problems in the background art, the present application aims to provide a positive electrode sheet and an electrochemical cell having a higher volumetric energy density and better cycle performance.
In order to achieve the above object, in one aspect of the present application, the present application provides a positive electrode sheet including a positive electrode current collector and a positive electrode membrane, the positive electrode membrane being disposed on the positive electrode current collector and including a positive electrode active material, a conductive agent, and a binder. The positive active material comprises a Prussian blue material, and the molecular formula of the Prussian blue material is AxMz[M′(CN)6]yWherein, A is one or more of alkali metal ions and alkaline earth metal ions, M is transition metal, M' is transition metal, x is more than 0 and less than or equal to 2, y is more than 0 and less than or equal to 1, z is more than 0 and less than or equal to 1, the particle size D50 of the Prussian blue material is 50 nm-10 mu M, and the porosity of the anode membrane is 10-50%.
In another aspect of the present application, there is provided an electrochemical cell comprising a positive electrode sheet according to one aspect of the present application.
Compared with the prior art, the application at least comprises the following beneficial effects:
the positive plate can ensure that the electrochemical cell has better cycle performance and higher volume energy density, and is suitable for large-scale production.
Drawings
FIG. 1 is a cycle performance curve for example 1 and comparative example 2;
fig. 2 is a cycle performance curve for example 1 and comparative example 4.
Detailed Description
The positive electrode sheet and the electrochemical cell according to the present application will be described in detail below.
The positive electrode sheet according to the first aspect of the present application is first explained.
The positive plate comprises a positive current collector and a positive diaphragm, wherein the positive diaphragm is arranged on the positive current collectorThe positive electrode current collector comprises a positive electrode active material, a conductive agent and a binder, wherein the positive electrode active material comprises a Prussian blue material, and the molecular formula of the Prussian blue material is AxMz[M′(CN)6]yWherein A is one or more of alkali metal cations and alkaline earth metal cations, M is transition metal, M' is transition metal, x is more than 0 and less than or equal to 2, y is more than 0 and less than or equal to 1, z is more than 0 and less than or equal to 1, the porosity of the positive electrode membrane is 10-50%, and the particle size D50 of the Prussian blue material is 50 nm-10 μ M.
In the positive electrode sheet according to the first aspect of the present application, preferably, a may be selected from Li+、Na+、K+、Mg2+、Ca2+Further preferably, A may be selected from Li+、Na+、K+One or more of the above; even more preferably, A may be selected from Li+、Na+One or two of them. Preferably, M may be selected from one of Mn, Fe, Co, Ni, Cu, Zn, V, Cr. Preferably, M' may be selected from one of Mn, Fe, Co, Ni, Cu, Zn, V, Cr.
In the positive electrode sheet according to the first aspect of the present application, when the porosity of the positive electrode sheet is large, the electrolyte can sufficiently infiltrate the prussian blue-based material particles, which is advantageous for the performance of the electrochemical cell. However, when the porosity of the positive electrode membrane is too high, more prussian blue material particles are directly exposed in the electrolyte in the long-term circulation process of the electrochemical cell, so that the probability of side reaction with the electrolyte is increased, and the circulation performance of the electrochemical cell is poor. In addition, when the porosity of the positive electrode membrane is too large, the volumetric energy density of the electrochemical cell is low, and meanwhile, due to the fact that the prussian blue material particles are not in close contact with each other, conduction of electrons between the prussian blue material particles is hindered, and the performance is also adversely affected. Therefore, the porosity of the positive electrode sheet is preferably controlled to 50% or less. When the porosity of the positive electrode membrane is low, the Prussian blue material particles are in close contact, conduction of electrons among the Prussian blue material particles is facilitated, and the volume energy density of the electrochemical cell is increased. If the porosity is too small, on one hand, the wettability of the electrolyte to prussian blue material particles is poor, and the transmission of ions in the positive plate is blocked, so that the cycle performance of the electrochemical cell is reduced; on the other hand, when the porosity is too small, the positive electrode sheet generally requires a large pressure during cold pressing, and the positive electrode sheet may be broken at a fold during a winding process in the electrochemical cell production process or during charge and discharge of the electrochemical cell due to the overpressure, thereby deteriorating the performance of the electrochemical cell. Therefore, the porosity of the positive electrode sheet is preferably controlled to 10% or more. The porosity of the positive diaphragm can be controlled by adjusting the cold pressing pressure in the preparation process of the pole piece, the grain size and the content of the active material and the like.
In the positive electrode sheet according to the first aspect of the present application, preferably, the porosity of the positive electrode sheet is 15% to 35%.
In the positive electrode sheet according to the first aspect of the present invention, when the particle size of the prussian blue material is small, the prussian blue material can be sufficiently impregnated with the electrolyte, and ions can be freely extracted and inserted. However, the particle size is too small, and stacking gaps among prussian blue material particles are large, so that the porosity of the positive electrode membrane is large, on one hand, the volume energy density is reduced, on the other hand, the prussian blue material particles are not in close contact, and meanwhile, due to the poor conductivity of the prussian blue material, a good conductive network is difficult to form among the prussian blue material particles, so that the capacity exertion of the electrochemical cell is influenced. Therefore, the particle size D50 of the prussian blue material is preferably controlled to be 50nm or more. The porosity of the positive electrode membrane can be reduced by increasing the particle size of the Prussian blue material, so that the Prussian blue material particles are in closer contact, the volume energy density is increased, and a good conductive network is established among the Prussian blue material particles, so that the electronic conduction among the particles is facilitated, and the electrochemical cell has better cycle performance. However, the prussian blue material has an excessively large particle size, and the diffusion path of ions in the prussian blue material is extended, which is not favorable for the desorption of ions, resulting in the degradation of the performance of the electrochemical cell. Therefore, the particle diameter D50 of the prussian blue material is preferably controlled to 10 μm or less.
In the positive electrode sheet according to the first aspect of the present application, the particle diameter D50 of the prussian blue material is preferably 500nm to 5 μm.
In the positive electrode sheet according to the first aspect of the present application, if the content of the prussian blue-based material is small, the volume energy density of the electrochemical cell is affected, and the porosity of the positive electrode sheet is also affected. Preferably, the content of the prussian blue material is 70% or more of the total mass of the positive electrode membrane, and more preferably, the content of the prussian blue material is 80% or more of the total mass of the positive electrode membrane.
In the positive electrode sheet according to the first aspect of the present application, other conventional positive electrode active materials may be further included in the positive electrode sheet.
In the positive plate according to the first aspect of the present application, the excessively low compaction density of the positive plate may cause the excessively low volumetric energy density of the electrochemical cell, which is not favorable for the overall design of the product and is difficult to meet the actual use requirement, and the excessively high compaction density of the positive plate may cause the positive plate to be over-pressurized, which may affect the infiltration of the electrolyte into the prussian blue material. Preferably, the compacted density of the positive electrode membrane is 0.8g/cm3～2.0g/cm3Further preferably, the compacted density of the positive electrode membrane sheet is 1.0g/cm3～1.5g/cm3。
In the positive electrode sheet according to the first aspect of the present application, the type of the binder is not particularly limited, and may be selected according to actual needs. Specifically, the binder may be one or more selected from oil-soluble binders and water-soluble binders.
In the positive electrode sheet according to the first aspect of the present application, the type of the oil-soluble binder is not particularly limited, and may be selected according to actual needs. Preferably, the oil-soluble binder can be selected from one or more of a vinylidene fluoride monomer homopolymer and a copolymer of a vinylidene fluoride monomer and a fluorine-containing vinyl monomer. The type of the copolymer of the vinylidene fluoride-based monomer and the fluorine-containing vinyl monomer is not particularly limited, and can be selected according to actual requirements. Specifically, the copolymer of the vinylidene fluoride-based monomer and the fluorine-containing vinyl monomer can be one or more selected from vinylidene fluoride-hexafluoropropylene copolymer, vinylidene fluoride-trifluoroethylene copolymer, vinylidene fluoride-chlorotrifluoroethylene copolymer, vinylidene fluoride-tetrafluoroethylene copolymer, vinylidene fluoride-trifluoroethylene-chlorovinylidene fluoride copolymer and tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride copolymer.
In the positive electrode sheet according to the first aspect of the present application, the kind of the water-soluble binder is not particularly limited, and may be selected according to actual needs. Preferably, the water-soluble binder can be one or more selected from styrene butadiene rubber, sodium carboxymethylcellulose, sodium alginate, polyacrylic acid and polytetrafluoroethylene.
In the positive electrode sheet according to the first aspect of the present application, the kind of the conductive agent is not particularly limited, and may be selected according to actual needs. Specifically, the conductive agent may be one or more selected from conductive carbon black (SuperP, Super S), ketjen black, acetylene black, conductive graphite, carbon nanotubes, and carbon nanofibers.
In the positive electrode sheet according to the first aspect of the present application, the kind of the positive electrode current collector is not particularly limited, and may be selected according to actual needs. Specifically, the positive electrode current collector may be selected from one of an aluminum foil, a porous aluminum foil, a stainless steel foil, and a porous stainless steel foil.
In the positive electrode sheet according to the first aspect of the present application, the method for producing the positive electrode sheet is not particularly limited, and a conventional method for producing a positive electrode sheet may be employed. Specifically, the prussian blue material, the conductive agent and the binder are mixed in a solvent according to a certain proportion to prepare positive electrode slurry, then the positive electrode slurry is coated on a positive electrode current collector, and finally the positive electrode sheet is prepared through the working procedures of drying, cold pressing and the like.
Next, an electrochemical cell according to the second aspect of the present application will be described.
An electrochemical cell according to the second aspect of the present application comprises a positive electrode sheet according to the first aspect of the present application.
In the electrochemical cell according to the second aspect of the present application, the electrochemical cell may further include a negative electrode sheet, an electrolyte, a separator, and the like.
In the electrochemical cell according to the second aspect of the present application, the electrochemical cell may be a lithium ion cell, a sodium ion cell, a potassium ion cell, a zinc ion cell, or an aluminum ion cell. In the embodiments of the present application, only the embodiment in which the electrochemical cell is a sodium ion cell is shown, but the present application is not limited thereto.
In the sodium ion battery, the negative electrode sheet may include a negative electrode current collector and a negative electrode membrane disposed on the negative electrode current collector and containing a negative electrode active material. The negative active material can be one or more selected from carbon materials, alloy materials, transition metal oxides and sulfides, phosphorus-based materials and titanate materials. Specifically, the carbon material may be one or more selected from hard carbon, soft carbon, amorphous carbon, and a nano-structured carbon material; the alloy material can be selected from one or more of Si, Ge, Sn, Pb and Sb; the transition metal oxides and sulfides have the general formula MxNyWherein M is one or more of Fe, Co, Ni, Cu, Mn, Sn, Mo, Sb and V, and N is O or S; the phosphorus-based material can be one or more of red phosphorus, white phosphorus and black phosphorus; the titanate material may be selected from Na2Ti3O7、Na2Ti6O13、Na4Ti5O12、Li4Ti5O12、NaTi2(PO4)3One or more of them.
In the sodium ion battery, the negative electrode sheet further comprises a conductive agent and a binder, and the types of the conductive agent and the binder are not particularly limited and can be selected according to actual requirements.
In a sodium ion battery, the electrolyte may be a liquid electrolyte, which may include a sodium salt, an organic solvent, and optional additives. The type of the sodium salt is not particularly limited, and can be selected according to actual requirements. Specifically, the sodium salt may be selected from sodium hexafluorophosphate (NaPF)6) Sodium perchlorate (NaClO)4) Sodium hexafluoroborate (NaBF)6) One or more of sodium trifluoromethanesulfonate and sodium trifluoromethanesulfonate (NaTFSI). The kind of the organic solvent is not particularly limited, and may be selected according to actual requirements. Specifically, the organic solvent may be one or more selected from Ethylene Carbonate (EC), Propylene Carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), and Ethyl Methyl Carbonate (EMC). The kind of the additive is not particularly limited, and the additive can be selectively added according to actual requirements.
In the sodium ion battery, the material of the isolation membrane is not limited and can be selected according to actual requirements. Specifically, the isolating film can be one or more of polypropylene film, polyethylene/polypropylene/polyethylene composite film, non-woven fabric film and glass fiber film.
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.
The sodium ion batteries of examples 1 to 9 and comparative examples 1 to 4 were each prepared as follows.
(1) Preparation of positive plate
Mixing Prussian blue material Na2MnFe(CN)6The conductive carbon black serving as a conductive agent and polyvinylidene fluoride (PVDF) serving as an oil-soluble binder are fully mixed according to the weight ratio of 80:10:10, then the mixture is added into an organic solvent N-methyl pyrrolidone (NMP), and the mixture is stirred uniformly to prepare anode slurry; uniformly coating the positive electrode slurry on the surface of an aluminum foil of a positive electrode current collector, and drying at 100 ℃ to obtain an initial positive plate; and finally, cold pressing the obtained initial positive plate by using a cold press to obtain the positive plate.
(2) Preparation of negative plate
Mixing the cathode active material hard carbon, binder Styrene Butadiene Rubber (SBR) and conductive carbon black serving as a conductive agent with solvent deionized water according to the weight ratio of 90:5:5, and uniformly stirring to obtain cathode slurry; and then uniformly coating the negative electrode slurry on a copper foil of a negative current collector, and then drying, cold pressing and stripping to obtain the negative plate.
(3) Preparation of the electrolyte
Mixing Ethylene Carbonate (EC) and dimethyl carbonate (DMC) according to a volume ratio of 1:1, and then fully drying sodium salt NaClO4Dissolving in mixed organic solvent to obtain electrolyte solution containing NaClO4The concentration of (2) is 1 mol/L.
(4) Preparation of the separator
A conventional polypropylene (PP) film was used as the separator.
(5) Preparation of sodium ion battery
And winding the positive plate, the negative plate and the isolating film to prepare a battery core, then filling the battery core into a battery packaging shell, then injecting electrolyte, and preparing the sodium ion battery by processes of formation, standing and the like.
The following describes the testing process of the sodium ion battery.
(1) Porosity test of positive membrane
The apparent density and the true density of the positive membrane are respectively tested by referring to the national standard GB/T24542 and 2009 iron ore determination, and then the porosity of the positive membrane is calculated, wherein the test and the specific calculation method are as follows: firstly, calculating the apparent density of the positive membrane according to the Archimedes drainage method principle, and recording the apparent density as rhoa(ii) a The positive diaphragm is then tested for true density using a true densitometer device, denoted as ρ.
Porosity P ═ of the positive electrode film (ρ - ρ)a)/ρ×100％。
(2) Cycle performance testing of sodium ion batteries
At 25 ℃, charging the sodium ion battery to a voltage of 4.0V at a constant current of 1C multiplying power, then charging to a current of 0.2C at a constant voltage of 4.0V, then standing for 5min, discharging to a voltage of 1.9V at a constant current of 1C multiplying power, and then standing for 5min, wherein the discharge capacity is recorded as the discharge capacity of the 1 st cycle of the sodium ion battery. And (3) carrying out 100-cycle charge and discharge tests on the sodium-ion battery according to the method, and detecting to obtain the discharge capacity of the 100 th cycle. Each group tested 4 sodium ion cells and the average was taken.
The capacity retention (%) after the sodium-ion battery was cycled 100 times was equal to the discharge capacity of the sodium-ion battery at 100 th cycle/discharge capacity of the lithium-ion battery at 1 st cycle × 100%.
(3) Volumetric energy density test of sodium ion battery
The capacity of each sodium ion battery is set to be 1Ah, then the actual volume of each sodium ion battery is tested according to the Archimedes drainage principle and recorded as V, and the average working voltage U of each sodium ion battery is 3.4V.
The volumetric energy density (Wh/L) of a sodium-ion battery is (the capacity (Ah) of the sodium-ion battery × the average operating voltage (V) of the sodium-ion battery))/the actual volume V (L) of the sodium-ion battery.
TABLE 1 parameters and results of Performance tests for examples 1-9 and comparative examples 1-4
Examples 1 to 5 and comparative examples 1 to 2 are the influence of the porosity of the positive electrode membrane on the performance of the sodium ion battery when the particle size of the prussian blue material is fixed. In comparative example 1, the porosity of the positive electrode membrane is too low, and although the sodium ion battery has a higher volume energy density, the cycle performance of the sodium ion battery is poor, and the whole sodium ion battery is difficult to meet the actual use requirement, because the too low porosity of the positive electrode membrane means that prussian blue material particles are stacked in a tighter manner, the occupied volume is smaller under the same cell capacity design, and the sodium ion battery has a higher volume energy density, but when the porosity of the positive electrode membrane is too low, the electrolyte infiltrates the prussian blue material particles slowly, and the transmission of sodium ions in the positive electrode membrane is hindered, so that the cycle performance of the sodium ion battery is poor. In addition, when the porosity of the positive electrode membrane is too low, the prussian blue material needs to bear large pressure during cold pressing, so that the positive electrode membrane is easy to be overpressured, and after the positive electrode membrane is wound into a battery cell, local fracture is easy to occur in the crease position in the charging and discharging process, so that the cycle performance is further deteriorated. As the porosity of the positive electrode membrane increased, the cycle performance of the sodium ion battery was improved in examples 1 to 5, but it is understood that the volumetric energy density of the sodium ion battery was slightly decreased, and the whole of the sodium ion battery could meet the demand for practical use. However, if the porosity of the positive electrode membrane is too high, such as in comparative example 2, the volumetric energy density and the cycle performance of the sodium ion battery are seriously affected, because when the porosity of the positive electrode membrane is too high, although the electrolyte can sufficiently infiltrate the prussian blue material particles, the contact between the prussian blue material particles is not tight enough, and the conduction of electrons between the prussian blue material particles is affected. In addition, in the long-term circulation process, the porosity of the positive electrode membrane is too high, more prussian blue material particle surfaces are directly exposed in the electrolyte, and the probability of side reaction with the electrolyte is increased. As can be seen from the analysis of fig. 1, the capacity protection rate of the sodium-ion battery in example 1 after 100 cycles is 93%, while the capacity retention rate of the sodium-ion battery in comparative example 2 after 100 cycles is only 78%.
Examples 1, 6 to 9, and 3 to 4 are effects of the particle size of the prussian blue material on the performance of the sodium ion battery when the porosity of the positive electrode membrane is fixed. In comparative example 3, the prussian blue type material was too small in particle size, the sodium ion battery had a low volumetric energy density, and the sodium ion battery had poor cycle performance because when the particle size of the prussian blue type material was too small, the specific surface area thereof was generally large, and thus the surface exposed to the electrolyte was more, the probability of side reaction with the electrolyte was increased, and the cycle performance of the sodium ion battery was deteriorated, and at the same time, the small particle size prussian blue type material was not closely stacked, and the volumetric energy density of the sodium ion battery was still low although the pressure at cold pressing was close to the pressure limit at the particle size. When the particle size of the prussian blue material is gradually increased, for example, in example 1 and examples 6 to 9, the prussian blue material can be stacked more tightly by increasing the cold pressing pressure, which is beneficial to establishing a good conductive network, thus being beneficial to electron conduction between particles, enabling the sodium-ion battery to have better cycle performance, and enabling the sodium-ion battery to have higher volume energy density. However, when the particle size of the prussian blue-based material is excessively large, such as in comparative example 4, the diffusion path of sodium ions in the prussian blue-based material is extended due to the large particle size of the individual prussian blue-based material, thereby causing deterioration in the cycle performance of the sodium ion battery. As can be seen from the analysis of fig. 2, the capacity retention rate of the sodium-ion battery after 100 cycles in example 1 is 93%, while the capacity retention rate of the sodium-ion battery after 100 cycles in comparative example 4 is only 82%.
To sum up, the positive plate of this application can guarantee that sodium ion battery has when better cycling performance compromise and have higher volume energy density, is fit for large-scale production.
Claims (9)
1. A sodium ion battery includes a positive electrode sheet;
the positive electrode sheet includes:
a positive current collector; and
the positive electrode diaphragm is arranged on the positive electrode current collector and comprises a positive electrode active material, a conductive agent and a binder;
it is characterized in that the preparation method is characterized in that,
the positive active material comprises a Prussian blue material, and the molecular formula of the Prussian blue material is AxMz[M′(CN)6]yWherein, A is one or more of alkali metal ions and alkaline earth metal ions, M is transition metal, M' is transition metal, x is more than 0 and less than or equal to 2, y is more than 0 and less than or equal to 1, and z is more than 0 and less than or equal to 1;
the particle size D50 of the Prussian blue material is 500 nm-10 mu m;
the porosity of the positive membrane is 15-35%.
2. The sodium-ion battery of claim 1,
a is selected from Li+、Na+、K+、Mg2+、Ca2+One or more of the above;
m is selected from one of Mn, Fe, Co, Ni, Cu, Zn, V and Cr;
m' is selected from one of Mn, Fe, Co, Ni, Cu, Zn, V and Cr.
3. The sodium ion battery according to claim 1, wherein the particle size D50 of the prussian blue material is 500nm to 5 μm.
4. The sodium ion battery of claim 1, wherein the positive electrode membrane sheet has a compacted density of 0.8g/cm3～2.0g/cm3。
5. The sodium ion battery of claim 1, wherein the positive electrode membrane sheet has a compacted density of 1.0g/cm3～1.5g/cm3。
6. The sodium-ion battery of claim 1, wherein the binder is selected from one or more of oil-soluble binders and water-soluble binders.
7. The sodium-ion battery of claim 1, wherein the conductive agent is selected from one or more of conductive carbon black, ketjen black, acetylene black, conductive graphite, carbon nanotubes, and carbon nanofibers.
8. The sodium-ion battery according to claim 1, wherein the prussian blue-based material is contained in an amount of 70% or more of the total mass of the positive electrode membrane.
9. The sodium-ion battery according to claim 1, wherein the prussian blue-based material is contained in an amount of 80% or more of the total mass of the positive electrode membrane.
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| CN105990567A (en) * | 2015-02-09 | 2016-10-05 | 中国科学院宁波材料技术与工程研究所 | Preparation method of prussian blue analogue nano-material and use of prussian blue analogue in sodium-ion battery |
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