CN109841832A - Positive plate and electrochemical cell - Google Patents
Positive plate and electrochemical cell Download PDFInfo
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- CN109841832A CN109841832A CN201711226486.0A CN201711226486A CN109841832A CN 109841832 A CN109841832 A CN 109841832A CN 201711226486 A CN201711226486 A CN 201711226486A CN 109841832 A CN109841832 A CN 109841832A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E60/10—Energy storage using batteries
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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
This application involves field of batteries more particularly to a kind of positive plates and electrochemical cell.
Background technique
Prussian blue (Prussian Blue Analogue, PBA) material because have specific capacity is high, voltage platform is high,
The advantages such as at low cost are the positive electrodes for obtaining extensive concern in recent years.Prussian blue material is during the preparation process because of ion
Reaction speed is fast, and the particle size generally yielded is smaller (generally nanoscale or micron order), thus makes to be difficult to press between particle
It is real, the foundation not only bad for conductive network between particle in this way, while the volume energy density of battery can be also reduced, thus not
Conducive to the whole design of product, thus how to take into account the volume energy density of battery and performance to be that prussian blue material is practical answer
With one of problem in need of consideration.
Summary of the invention
In view of the problems in the background art, the application is designed to provide a kind of positive plate and electrochemical cell,
The electrochemical cell volume energy density with higher and preferable cycle performance.
In order to achieve the above object, in the one side of the application, this application provides a kind of positive plates comprising anode collection
Fluid and positive diaphragm, the anode diaphragm are set on the plus plate current-collecting body and including positive electrode active materials, conductive agent
And binder.The positive electrode active materials include prussian blue material, and the molecular formula of the prussian blue material is AxMz
[M′(CN)6]y, wherein A is one or more of alkali metal ion, alkaline-earth metal ions, and M is transition metal, and M ' is transition
Metal, 0 < x≤2,0 < y≤1,0 z≤1 <, the partial size D50 of the prussian blue material is 50nm~10 μm, the anode
The porosity of diaphragm is 10%~50%.
In the another aspect of the application, this application provides a kind of electrochemical cells comprising described in the application one side
Positive plate.
Compared with the existing technology, the application include at least it is following the utility model has the advantages that
The positive plate of the application is taken into account while can guaranteeing electrochemical cell with preferable cycle performance with higher
Volume energy density, be suitble to large-scale production.
Detailed description of the invention
Fig. 1 is the cycle performance curve of embodiment 1 and comparative example 2；
Fig. 2 is the cycle performance curve of embodiment 1 and comparative example 4.
Specific embodiment
The following detailed description of the positive plate and electrochemical cell according to the application.
Illustrate the positive plate according to the application first aspect first.
Positive plate according to the application first aspect includes plus plate current-collecting body and positive diaphragm, the anode diaphragm setting
In on the plus plate current-collecting body and including positive electrode active materials, conductive agent and binder, the positive electrode active materials include general
Shandong scholar's indigo plant class material, the molecular formula of the prussian blue material are AxMz[M′(CN)6]y, wherein A be alkali metal cation,
One or more of alkaline earth metal cation, M are transition metal, and M ' is transition metal, 0 < x≤2,0 < y≤1,0 < z≤
1, the porosity of the anode diaphragm is 10%~50%, and the partial size D50 of the prussian blue material is 50nm~10 μm.
In the positive plate according to the application first aspect, it is preferable that A can be selected from Li+、Na+、K+、Mg2+、Ca2+In
One or more, it is further preferred that A can be selected from Li+、Na+、K+One or more of；It is further preferred that A is optional
From Li+、Na+One or both of.Preferably, M can be selected from one of Mn, Fe, Co, Ni, Cu, Zn, V, Cr.Preferably, M '
It can be selected from one of Mn, Fe, Co, Ni, Cu, Zn, V, Cr.
In the positive plate according to the application first aspect, when the porosity of positive diaphragm is larger, electrolyte can
Adequately to be infiltrated to prussian blue material granule, this plays the performance of electrochemical cell advantageous.But positive diaphragm
Porosity it is excessive when, in the long-term cyclic process of electrochemical cell, more prussian blue material granules surface is direct
Exposure in the electrolytic solution, increases the probability that side reaction occurs with electrolyte, poor so as to cause the cycle performance of electrochemical cell.
In addition, when the porosity of positive diaphragm is excessive, the volume energy density of electrochemical cell is lower, simultaneously because prussian blue
Contact between material granule is not close, and conduction of the electronics between prussian blue material granule is obstructed, and can also make to performance
At adverse effect.Therefore, the porosity of positive diaphragm preferably controls below 50%.It is general when the porosity of positive diaphragm
It is contacted between the scholar's indigo plant class material granule of Shandong relatively closely, is conducive to conduction of the electronics between prussian blue material granule, simultaneously
The volume energy density of electrochemical cell increases.If but porosity is too small, on the one hand, electrolyte is to prussian blue material granule
Wellability be deteriorated, ion transmit in positive plate and is obstructed, and the cycle performance that will lead to electrochemical cell declines；On the other hand,
When porosity is too small, positive plate usually requires larger pressure in cold pressure procedure, and positive plate may cause because of over-voltage in electrochemistry
It is broken at folding line in the rolling step of cell production process or in electrochemical cell charge and discharge process, thus to electrification
The performance for learning battery causes to deteriorate.Therefore, the porosity of positive diaphragm is preferably controlled 10% or more.The porosity of positive diaphragm can
To be controlled by the partial size for adjusting the cold pressing pressure in pole piece preparation process, active material and content etc..
In the positive plate according to the application first aspect, it is preferable that the porosity of the anode diaphragm is 15%
~35%.
In the positive plate according to the application first aspect, when the partial size of prussian blue material is smaller, electrolysis
Liquid can sufficiently infiltrate it, while ion can also free deintercalation.But partial size is too small, prussian blue material granule it
Between stacking gap it is larger, cause the porosity of positive diaphragm larger, on the one hand can reduce volume energy density, on the other hand also
The contact between prussian blue material granule can be made not close, while because of prussian blue material poorly conductive itself, can be made
Good conductive network is formed at being difficult between prussian blue material granule, so that the capacity for influencing electrochemical cell plays.
Therefore, the partial size D50 of prussian blue material is preferably controlled in 50nm or more.And the partial size for increasing prussian blue material can subtract
The porosity of small anode diaphragm, keeps the contact between prussian blue material granule closer, increases volume energy density, simultaneously
It also helps and establishes good conductive network between prussian blue material granule, so that the electronics be conducive between particle passes
It leads, makes electrochemical cell that there is preferable cycle performance.But the partial size of prussian blue material is excessive, and ion is in diffusion wherein
Path extends, and is unfavorable for the deintercalation of ion, the performance of electrochemical cell is caused to decline.Therefore, the partial size of prussian blue material
D50 is preferably controlled at 10 μm or less.
In the positive plate according to the application first aspect, it is preferable that the partial size D50 of the prussian blue material
For 500nm~5 μm.
In the positive plate according to the application first aspect, if the content of prussian blue material is less, on the one hand
It will affect the volume energy density of electrochemical cell, on the other hand also will affect the porosity of positive diaphragm.Preferably, described general
The content of Shandong scholar's indigo plant class material is more than or equal to the 70% of the positive diaphragm gross mass, it is further preferred that described Prussian blue
The content of class material is more than or equal to the 80% of the positive diaphragm gross mass.
In the positive plate according to the application first aspect, it is described anode diaphragm in may also include it is other it is conventional just
Pole active material.
In the positive plate according to the application first aspect, the compacted density of positive diaphragm is too low to will cause electrochemistry
The volume energy density of battery is too low, is unfavorable for the whole design of product and is difficult to meet the actual needs, positive diaphragm
Compacted density is excessive, then causes positive plate by over-voltage, influence infiltration of the electrolyte to prussian blue material.Preferably, described
The compacted density of positive diaphragm is 0.8g/cm3~2.0g/cm3, it is further preferred that the compacted density of the anode diaphragm is
1.0g/cm3~1.5g/cm3。
In the positive plate according to the application first aspect, the type of the binder is not limited specifically, can
It is selected according to actual needs.Specifically, the binder can be selected from one of oil-soluble binder, water-soluble binder
Or it is several.
In the positive plate according to the application first aspect, the type of the oil-soluble binder is not limited specifically
System, can be selected according to actual needs.Preferably, the oil-soluble binder can be selected from vinylidene fluoride monomer homopolymers,
One or more of the copolymer of vinylidene fluoride monomer and fluorine-containing vinyl monomer.The vinylidene fluoride monomer with it is fluorine-containing
The type of the copolymer of vinyl monomer does not limit specifically, can be selected according to actual needs.Specifically, the inclined fluorine
The copolymer of vinyl monomer and fluorine-containing vinyl monomer can be selected from vinylidene fluoride-hexafluoropropylene copolymer, vinylidene-trifluoro
Ethylene copolymer, vinylidene-chlorotrifluoroethylene, skewed segregation, vinylidene-trifluoro second
One or more of alkene-chloro vinylidene fluoride copolymers, hexafluoropropylene (HFP)/tetrafluoroethylene (TFE)-vinylidene fluoride copolymers.
In the positive plate according to the application first aspect, the type of the water-soluble binder is not limited specifically
System, can be selected according to actual needs.Preferably, the water-soluble binder can be selected from butadiene-styrene rubber, carboxymethyl cellulose
One or more of sodium, sodium alginate, polyacrylic acid, polytetrafluoroethylene (PTFE).
In the positive plate according to the application first aspect, the type of the conductive agent is not limited specifically, can
It is selected according to actual needs.Specifically, the conductive agent can be selected from conductive black (SuperP, Super S), Ketjen black,
One or more of acetylene black, electrically conductive graphite, carbon nanotube, carbon nano-fiber.
In the positive plate according to the application first aspect, the type of the plus plate current-collecting body is not limited specifically
System, can be selected according to actual needs.Specifically, the plus plate current-collecting body can be selected from aluminium foil, porous aluminium foil, stainless steel foil,
One of porous stainless steel foil.
In the positive plate according to the application first aspect, the preparation method of the positive plate is not limited particularly
System, using the preparation method of conventional cathode piece.Specifically, can in a solvent by prussian blue material, conductive agent and
Binder, which is mixed in a certain ratio, is prepared into anode sizing agent, then presses anode sizing agent and is coated on plus plate current-collecting body, most passes through afterwards
It crosses the processes such as drying, cold pressing and is prepared into the positive plate.
Secondly explanation electrochemical cell according to the application second aspect.
Electrochemical cell according to the application second aspect includes the positive plate according to the application first aspect.
In the electrochemical cell according to the application second aspect, the electrochemical cell may also include negative electrode tab,
Electrolyte and isolation film etc..
In the electrochemical cell according to the application second aspect, the electrochemical cell can for lithium ion battery,
Sodium-ion battery, kalium ion battery, Zinc ion battery or aluminium ion battery.In embodiments herein, electrochemistry is only shown
Battery is the embodiment of sodium-ion battery, but the application is without being limited thereto.
In sodium-ion battery, negative electrode tab may include negative current collector and be set on negative current collector and contain cathode
The cathode membrane of active material.The negative electrode active material can be selected from carbon material, alloy material, transition metal oxide and vulcanization
One or more of object, phosphorous-based materials, titanate material.Specifically, the carbon material can be selected from hard carbon, soft carbon, amorphous
One or more of carbon, nanostructured carbon material；The alloy material can be selected from one of Si, Ge, Sn, Pb, Sb or several
The alloy material that kind is formed；The general formula of the transition metal oxide and sulfide is MxNy, wherein M be Fe, Co, Ni, Cu, Mn,
The one or more of Sn, Mo, Sb, V, N are O or S；The phosphorous-based materials can be selected from one of red phosphorus, white phosphorus, black phosphorus or several
Kind；The titanate material can be selected from Na2Ti3O7、Na2Ti6O13、Na4Ti5O12、Li4Ti5O12、NaTi2(PO4)3One of or
It is several.
In sodium-ion battery, the negative electrode tab further includes conductive agent and binder, the kind of the conductive agent and binder
Class does not limit specifically, can be selected according to actual needs.
In sodium-ion battery, the electrolyte can be liquid electrolyte, and the electrolyte may include sodium salt, organic solvent
And optional additive.The type of the sodium salt does not limit specifically, can be selected according to actual needs.Specifically,
The sodium salt can be selected from sodium hexafluoro phosphate (NaPF6), sodium perchlorate (NaClO4), hexafluoro Boratex (NaBF6), trifluoromethyl sulphur
One or more of sour sodium, trifluoromethane sulfonic acid imines sodium (NaTFSI).The type of the organic solvent does not limit specifically
System, can be selected according to actual needs.Specifically, the organic solvent can be selected from ethylene carbonate (EC), propene carbonate
(PC), one of dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC) or and several.The addition
The type of agent does not limit specifically, can selectively add according to actual needs.
In sodium-ion battery, the material of the isolation film is unrestricted, can be selected according to actual needs.Specifically
Ground, isolation film can be selected from polypropylene screen, polyethylene film, polyethylene/polypropylene/polyethylene composite membrane, non-woven membrane, glass fibers
Tie up one or more of film.
Below with reference to embodiment, the application is further described.It should be understood that these embodiments be merely to illustrate the application without
For limiting scope of the present application.
The sodium-ion battery of embodiment 1-9 and comparative example 1-4 are prepared by the following method.
(1) preparation of positive plate
By prussian blue material Na2MnFe(CN)6, conductive agent conductive carbon black, oil-soluble binder polyvinylidene fluoride
(PVDF) it by weight being sufficiently mixed for 80:10:10, is then added in organic solvent N-Methyl pyrrolidone (NMP), stirs
Anode sizing agent is prepared into after uniformly；Anode sizing agent is then coated uniformly on to the surface of plus plate current-collecting body aluminium foil, later again 100
It is dried at DEG C, obtains initial positive plate；Finally obtained initial positive plate is cold-pressed using cold press, obtains positive plate.
(2) preparation of negative electrode tab
By negative electrode active material hard carbon, binder butadiene-styrene rubber (SBR), conductive agent conductive carbon black according to weight ratio be 90:
5:5 is mixed with solvent deionized water, obtains negative electrode slurry after mixing evenly；Then negative electrode slurry is coated uniformly on negative pole currect collecting
On body copper foil, negative electrode tab is obtained by drying, cold pressing, slitting later.
(3) preparation of electrolyte
Ethylene carbonate (EC), dimethyl carbonate (DMC) are mixed according to volume ratio for 1:1, then will sufficiently be done
Dry sodium salt NaClO4It is dissolved in mixed organic solvents, obtains electrolyte, wherein NaClO4Concentration be 1mol/L.
(4) preparation of isolation film
Using conventional polypropylene (PP) film as isolation film.
(5) preparation of sodium-ion battery
Battery core is made by winding in positive plate, negative electrode tab and isolation film, then battery core is fitted into battery packages shell, it
After inject electrolyte, using chemical conversion, stand etc. techniques be made sodium-ion battery.
The test process of sodium-ion battery will be illustrated next.
(1) porosity test of positive diaphragm
Respectively referring to national standard " measurement of GB/T 24586-2009 iron ore apparent density, real density and porosity "
The apparent density and real density of positive diaphragm are tested, the porosity of positive diaphragm, test and specific calculation method are then calculated
It is as follows: to calculate the apparent density of positive diaphragm according to Archimedes's drainage principle first, be denoted as ρa；Then real density is used
Instrument equipment tests the real density of positive diaphragm, is denoted as ρ.
Porosity P=(ρ-the ρ of positive diaphragma)/ρ × 100%.
(2) the cycle performance test of sodium-ion battery
It with 1C multiplying power constant-current charge to voltage is 4.0V by sodium-ion battery, later with 4.0V constant-voltage charge at 25 DEG C
It is 0.2C to electric current, stands 5min later, be 1.9V with 1C multiplying power constant-current discharge to voltage, then stand 5min, this is followed for one
Ring charge and discharge process, this discharge capacity are denoted as the discharge capacity of sodium-ion battery the 1st time circulation.By sodium-ion battery according to
The above method carries out 100 cyclic charging and discharging tests, and detection obtains the discharge capacity of the 100th circulation.4 sodium of every group of test from
Sub- battery, is averaged.
Capacity retention ratio (%)=sodium-ion battery the 100th time electric discharge recycled after sodium-ion battery recycles 100 times is held
Discharge capacity × 100% of amount/lithium ion battery the 1st time circulation.
(3) the volume energy density test of sodium-ion battery
The capacity of sodium-ion battery is set as 1Ah, then tests sodium-ion battery according to Archimedes's drainage principle
Actual volume, and it is recorded as V, the average working voltage U of sodium-ion battery is 3.4V.
The volume energy density (Wh/L) of sodium-ion battery=(capacity (Ah) × sodium-ion battery of sodium-ion battery is flat
Equal operating voltage (V))/sodium-ion battery actual volume V (L).
The parameter and the performance test results of table 1 embodiment 1-9 and comparative example 1-4
When embodiment 1-5, comparative example 1-2 are that the partial size of prussian blue material is fixed, the porosity of positive diaphragm is to sodium
The influence of ion battery performance.In comparative example 1, the porosity of positive diaphragm is too low, although sodium-ion battery has higher volumes
Energy density, but the cycle performance of sodium-ion battery is poor, is integrally difficult to meet the actual needs, the reason is that, cathode film
The porosity of piece is too low to be meaned to stack in a manner of more close between prussian blue material granule, therefore identical battery core is held
Occupied volume is smaller under amount design, sodium-ion battery volume energy density with higher, but the porosity of positive diaphragm
When too low, electrolyte is slower to the infiltration of prussian blue material granule, and transmission of the sodium ion in positive plate is obstructed, to lead
Cause sodium-ion battery cycle performance poor.In addition, prussian blue material is needed in cold pressing when the porosity of positive diaphragm is too low
Larger pressure is born, causes positive plate easily by over-voltage, after being wound into battery core, folding line, which is in charge and discharge process, is easy hair
Raw local fracture, to further deteriorate cycle performance.With the increase of the porosity of positive diaphragm, in embodiment 1-5, sodium
The cycle performance of ion battery is improved, but it is understood that, the volume energy density of sodium-ion battery slightly reduces,
Entirety can satisfy the demand of actual use.If but the porosity of positive diaphragm is excessively high, such as comparative example 2, can seriously affect sodium
The volume energy density and cycle performance of ion battery, the reason is that, when the porosity of positive diaphragm is excessive, although electrolyte can
Contact defective tightness adequately to be infiltrated to prussian blue material granule, but between prussian blue material granule,
It will affect conduction of the electronics between prussian blue material granule.In addition, in long-term cyclic process, the hole of positive diaphragm
Rate is excessive, has more prussian blue material granules surface and is directly exposed in electrolyte, increases and pair occurs with electrolyte
The probability of reaction.In conjunction with Fig. 1 analysis it is found that in embodiment 1, the capacity protective rate after sodium-ion battery recycles 100 times is 93%,
And in comparative example 2, the capacity retention ratio after sodium-ion battery recycles 100 times is only 78%.
When embodiment 1, embodiment 6-9, comparative example 3-4 are that the porosity of positive diaphragm is fixed, prussian blue material
Influence of the partial size to sodium-ion battery performance.In comparative example 3, the partial size of prussian blue material is too small, the body of sodium-ion battery
Product energy density is lower, and the cycle performance of sodium-ion battery is poor, the reason is that, the partial size of prussian blue material is too small
When, specific surface area is usually larger, therefore the surface of exposure in the electrolytic solution is more, and the probability that side reaction occurs with electrolyte increases
Add, deteriorate the cycle performance of sodium-ion battery, at the same between the prussian blue material of small particle can not Close stack, although cold
Pressure is already close to the pressure limit under the partial size when pressure, but the volume energy density of sodium-ion battery is still lower.When general Shandong
When the partial size of scholar's indigo plant class material is gradually increased, such as in embodiment 1, embodiment 6-9, Pu Lu can be made by increasing cold pressing pressure
It is closer that scholar's indigo plant carrys out the stacking between material granule, is conducive to establish good conductive network, to be conducive between particle
Electronics conduction, makes sodium-ion battery have preferable cycle performance, while keeping sodium-ion battery volume energy with higher close
Degree.But when the partial size of prussian blue material is excessive, such as comparative example 4, due to the partial size ruler of single prussian blue material
Very little larger, sodium ion diffusion path in prussian blue material extends, and deteriorates so as to cause the cycle performance of sodium-ion battery.
It is analyzed in conjunction with Fig. 2 it is found that the capacity retention ratio after sodium-ion battery recycles 100 times is 93%, and comparative example 4 in embodiment 1
In, the capacity retention ratio after sodium-ion battery recycles 100 times is only 82%.
In conclusion the positive plate of the application can guarantee to take into account while sodium-ion battery has preferable cycle performance
Volume energy density with higher is suitble to large-scale production.
Claims (10)
1. a kind of positive plate, comprising:
Plus plate current-collecting body；And
Positive diaphragm is set on the plus plate current-collecting body and including positive electrode active materials, conductive agent and binder；
It is characterized in that,
The positive electrode active materials include prussian blue material, and the molecular formula of the prussian blue material is AxMz[M′
(CN)6]y, wherein A is one or more of alkali metal ion, alkaline-earth metal ions, and M is transition metal, and M ' is transition gold
Belong to, 0 < x≤2,0 < y≤1,0 z≤1 <；
The partial size D50 of the prussian blue material is 50nm~10 μm；
The porosity of the anode diaphragm is 10%~50%.
2. positive plate according to claim 1, which is characterized in that
A is selected from Li+、Na+、K+、Mg2+、Ca2+One or more of；
M is selected from one of Mn, Fe, Co, Ni, Cu, Zn, V, Cr；
M ' is selected from one of Mn, Fe, Co, Ni, Cu, Zn, V, Cr.
3. positive plate according to claim 1, which is characterized in that the porosity of the anode diaphragm is 15%~35%.
4. positive plate according to claim 1, which is characterized in that the partial size D50 of the Prussian blue material be 500nm~
5μm。
5. positive plate according to claim 1, which is characterized in that the compacted density of the anode diaphragm is 0.8g/cm3~
2.0g/cm3。
6. positive plate according to claim 4, which is characterized in that the compacted density of the anode diaphragm is 1.0g/cm3~
1.5g/cm3。
7. positive plate according to claim 1, which is characterized in that the binder is selected from oil-soluble binder, water solubility
One or more of binder.
8. positive plate according to claim 1, which is characterized in that the conductive agent is selected from conductive black, Ketjen black, acetylene
One or more of black, electrically conductive graphite, carbon nanotube, carbon nano-fiber.
9. positive plate according to claim 1, which is characterized in that the content of the prussian blue material is more than or equal to institute
State the 70% of positive diaphragm gross mass, it is preferable that the content of the prussian blue material is more than or equal to greatly the positive diaphragm
The 80% of gross mass.
10. a kind of electrochemical cell, which is characterized in that including positive plate according to claim 1 to 9.
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| CN112259730A (en) * | 2020-12-08 | 2021-01-22 | 江苏时代新能源科技有限公司 | Prussian blue transition metal cyanide, preparation method thereof, and related positive electrode plate, secondary battery, battery pack and device |
| CN113437261A (en) * | 2021-06-22 | 2021-09-24 | 中国电力科学研究院有限公司 | Prussian blue positive plate, sodium ion battery and preparation method |
| CN113488611A (en) * | 2021-06-24 | 2021-10-08 | 东莞塔菲尔新能源科技有限公司 | Electrode assembly and secondary battery |
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