CN108736010A - A kind of safe full phosphate sodium ion secondary battery - Google Patents
A kind of safe full phosphate sodium ion secondary battery Download PDFInfo
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- CN108736010A CN108736010A CN201710252586.4A CN201710252586A CN108736010A CN 108736010 A CN108736010 A CN 108736010A CN 201710252586 A CN201710252586 A CN 201710252586A CN 108736010 A CN108736010 A CN 108736010A
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- Prior art keywords
- phosphate
- ion secondary
- secondary battery
- sodium ion
- sodium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a kind of safe full phosphate sodium ion secondary batteries.The full phosphate sodium ion secondary battery selects positive and negative pole material of the phosphate compound with high heat stability as sodium ion secondary battery, and using non-combustible phosphate or phosphonic acid ester as electrolyte, the full phosphate sodium-ion battery cathode good compatibility formed, electrochemical window mouth width, the initial temperature of positive and negative polar decomghtion has been delayed, there is long cycle life, good chemical property and high safety.
Description
Technical field
The present invention relates to new energy materials and technical field of energy storage, more particularly to a kind of high safety, zero strain sodium ion two
Primary cell preparation method.
Background technology
In order to efficiently use the regenerative resources such as wind energy, solar energy, tide energy, low cost, the energy storage system of high safety by
To extensive concern.In recent years, sodium-ion battery is increasingly becoming grinding for energy storage field due to resourceful, lower-price characteristic
Study carefully hot spot.However, in order to preferably meet practical requirement, sodium-ion battery also needs to promote cycle life, high rate performance, peace
Full performance etc..
Phosphate compound has firm frame structure, to have higher cyclicity and safety, such as
NaFePO4、Na3V2(PO4)3、NaTi2(PO4)3Equal materials, usually have long circulation life, good high rate performance.However at present
Most of sodium ion secondary battery is had potential dangerous all using flammable carbonic ester as electrolyte.Grinding in recent years
Middle generally use aqueous solution is studied carefully to replace flammable phosphate electrolyte, if patent CN105489949A is with the aqueous solution containing zinc, sodium
As the electrolyte of sodium rechargeable battery, however aqueous solution electrochemical window is relatively narrow, hydrogen-oxygen be precipitated etc. side reactions and its to storage sodium electricity
The interaction of pole material can influence sodium-ion battery efficiency for charge-discharge and cyclical stability.Phosphate compounds usually have
Good anti-flammability, at present most of researchs prepare fire retardant or even non-ignitable lithium-ion electric as additive or cosolvent
Pond electrolyte.Such as United States Patent (USP) US6, the trimethyl phosphate of 589,697, US6,924,061, US6,589,697 reports, tricresyl phosphate
Phenyl ester, tributyl phosphate, the phosphoric acid esters such as trifluoroethyl phosphate reduce its combustibility as electrolysis additive.China
Patent CN200710052150.7 uses one or more of phosphates such as methyl-phosphoric acid dimethyl ester, ethyl phosphonic acid diethylester, second
Base dimethyl phosphate has obtained a kind of lithium-ion battery electrolytes of efficient low-poison and combustion-resisting as solvent additive or pure solvent.
However, phosphoric acid ester electrolyte is directly used in sodium-ion battery, it is narrow that there are electrochemical windows, not with anode material of lithium-ion battery
It is compatible, it is poor to the dissolubility of sodium salt the problems such as, currently without making pure solvent use in sodium-ion battery electrolyte.If can study
A kind of high safety, zero strain sodium ion secondary battery are provided, its potential safety problem is solved, it will certainly be pushed in energy storage field
High speed development.
Invention content
For the short problem with safety difference of cycle life existing for present sodium ion secondary battery, present invention selection has
Positive and negative anodes of the phosphate compound of high heat stability as sodium ion secondary battery, and made with non-combustible phosphate or phosphonate ester
For electrolyte, be prepared for a kind of high safety, long circulation life, good chemical property the complete secondary electricity of phosphate sodium ion
Pond.
The present invention provides such as following technical proposals：
A kind of safe full phosphate sodium ion secondary battery, including anode, cathode, diaphragm and electrolyte, feature exist
In：Positive active material is NaFePO4、Na3V2(PO4)3、Na2FeP2O7、Na2MnP2O7、Na2CoP2O7、Na7V3(P2O7)4,
Na2FePO4F、Na3V2(PO4)2F3、Na4Fe3(PO4)2(P2O7)、Na4Co3(PO4)2(P2O7) in one kind；Negative electrode active material
For NaTi2(PO4)3, Na2TiCr(PO4)3、NaZr2(PO4)3、Na1.5Fe0.5Ti1.5(PO4)3、TiP2O7In one kind；Described
Electrolyte is non-combustible phosphate or phosphonate species electrolyte containing sodium salt.
By said program, the anode pole piece is prepared by positive active material, conductive agent and binder, specific to make
Preparation Method is：Positive active material, conductive agent and binder are mixed in proportion, solvent is added and is tuned into slurry, is coated on
On aluminium foil, it is dried in vacuum overnight and can be obtained anode pole piece；
The cathode pole piece is prepared by negative electrode active material, conductive agent and binder, and specific preparation method is：
Negative electrode active material, conductive agent and binder are mixed in proportion, solvent is added and is tuned into slurry, is coated on aluminium foil, very
Sky, which is dried overnight, can be obtained cathode pole piece；
Wherein, the mass percent of positive active material, conductive agent and binder is 60~90%：5~20%：5~
20%, the mass percent of negative electrode active material, conductive agent and binder is 60~90%：5~20%：5~20%.
By said program, conductive agent is one or more of acetylene black, Ketjen black, Super P, and binder is poly- inclined two
One or more of vinyl fluoride, polytetrafluoroethylene (PTFE), sodium carboxymethylcellulose, poly- butadiene-styrene rubber, polyacrylic acid, sodium alginate,
Solvent is one kind in N-Methyl pyrrolidone, water.
By said program, vacuum drying temperature is 120 DEG C.
By said program, the structure of phosphate or phosphonate species is (RO)3P=O or R (RO2) P=O, R be phenyl or
Carbon chain lengths be 1-6 lower alkyl groups or halogenated alkyl, preferably triphenyl phosphate (TPP), trimethyl phosphate (TMP),
Triethyl phosphate (TEP), dimethyl methyl phosphonate (DMMP), bis- (2,2,2- trifluoroethyls) methyl phosphorodithioates (TFMP) etc..
By said program, sodium salt is sodium perchlorate, sodium hexafluoro phosphate, double trifluoromethanesulfonimide sodium (NaTFSI), three
One or more of fluoromethane sodium sulfonate (NaFS), preferably double trifluoromethanesulfonimide sodium, trifluoromethayl sulfonic acid sodium.
By said program, a concentration of 0.5~3 mole every liter of the sodium salt.
By said program, diaphragm is polyimide film, glass fibre membrane, polyacrylonitrile film, polyethylene terephthalate
Film, polyether-ether-ketone film, one kind in polytetrafluoroethylene film or composite membrane.
By said program, the positive and negative highly preferred combination (anode/cathode) is as follows：Na3V2(PO4)3/NaTi2(PO4)3,
Na3V2(PO4)3/Na2TiCr(PO4)3、Na3V2(PO4)2F3/NaTi2(PO4)3、Na3V2(PO4)3/Na1.5Fe0.5Ti1.5(PO4)3、
Na2FeP2O7//NaTi2(PO4)3、NaFePO4/TiP2O7。
The beneficial effects of the invention are as follows：
The present invention directly does electrolyte with non-combustible phosphate ester (phosphonate ester), and without using electrolysis additive, cooperation is just
The full phosphate sodium ion secondary battery that the selection of pole, negative material and sodium salt obtains and cathode good compatibility, electrochemical window
Width has extended cycle life, and has delayed the initial temperature of positive and negative polar decomghtion, improves the safety of battery.
Further preferably the phosphate positive and negative pole material with similar and opposite volume change, no big volume change are drawn
The structure risen is destroyed, it is ensured that the stability of the dimensional stability of battery discharge procedure, full battery structure is high, long lifespan.
Description of the drawings
Fig. 1 is the changes in crystal structure after the full phosphate sodium-ion battery charging of embodiment 1；
Fig. 2 is the DSC curve after the full phosphate sodium-ion battery charging of embodiment 1 and comparative example 1；
Fig. 3 is the constant current cycle figure of the sodium-ion battery of embodiment 1；
Fig. 4 is cyclic voltammetry curve of the electrolyte on platinum electrode；
Fig. 5 is all charging curves of head of comparative example 2；
Fig. 6 is the sodium-ion battery constant current cycle figure of embodiment 3；
Fig. 7 is the sodium-ion battery constant current cycle figure of embodiment 4.
Specific implementation mode
The embodiments described below are only a part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment belongs to protection scope of the present invention.
Embodiment one：
With Na3V2(PO4)3For positive active material, acetylene black is conductive agent, and polytetrafluoroethylene (PTFE) is binder, in mass ratio
It is 70：20：10 ratio is uniformly mixed, and N-Methyl pyrrolidone is added and is tuned into slurry, is coated on aluminium foil, and 120 DEG C of vacuum are dry
It is dry to can be obtained anode pole piece overnight.With NaTi2(PO4)3For negative electrode active material, acetylene black is conductive agent, and polytetrafluoroethylene (PTFE) is
Binder is in mass ratio 70：20：10 ratio is uniformly mixed, and N-Methyl pyrrolidone is added and is tuned into slurry, is coated on aluminium foil
On, 120 DEG C are dried in vacuum overnight and can be obtained cathode pole piece.
Using the trimethyl phosphate of the NaFS containing 1M as electrolyte, glass fiber filter is diaphragm, and above-mentioned material is assembled into
Full battery carries out electrochemical property test on charge and discharge instrument, does cyclic voltammetry scan of the electrolyte on platinum electrode.Battery follows
Ring test shows that the battery has good cycle performance (see Fig. 3), and circulation volume conservation rate still has 77% within 1000 weeks.Cycle
Voltammetric scan shows that electrolyte, without apparent peak, shows its electrochemistry between 0-4.3V within the scope of scanning voltage (see Fig. 4)
It can stablize.
After the battery of Charging state is disassembled, differential scanning calorimetry is carried out to positive and negative anodes pole piece respectively and X-ray diffraction is surveyed
It tries (seeing Fig. 2 and Fig. 1 respectively).Differential scanning calorimetry test shows after charge and discharge (under charged state), uses trimethyl phosphate electricity
The vanadium phosphate sodium material heat production temperature for solving liquid is 323 DEG C, and titanium phosphate sodium material heat production temperature is 295 DEG C, and quantity of heat production also phase
It should reduce, show great safety.Simulation calculating is carried out with the data that X-ray diffraction is tested, shows to use phosphorus
Overall volume variation is only 0.33% after the battery positive/negative plate charging of acid esters electrolyte.Comparative example 1：It is identical as experimental example, no
It is the characterization using pole piece when conventional carbonic ester electrolyte progress charge and discharge and Charging state with place.
Differential scanning calorimetry test shows that the vanadium phosphate sodium material heat production temperature using conventional carbonic ester electrolyte is 330
DEG C, titanium phosphate sodium material heat production temperature is 417 DEG C.Simulation calculating is carried out with the data that X-ray diffraction is tested, shows to use
After the battery pole piece charging of carbonic ester electrolyte, overall volume variation is 2.59%.Compared with embodiment one, comparative example heat production
Temperature relatively shifts to an earlier date, and full battery volume change is larger, is unfavorable for safety and the cyclicity of battery.Comparative example 2：Such as embodiment
1 is identical, the difference is that cathode selects hard charcoal.
Comparative example 3：It is same as Example 1, the difference is that cathode selects metallic tin.
The battery charging and discharging of comparative example 2 and comparative example 3 show battery can not charge and discharge, illustrate pure phosphoric acid trimethyl be electrolysed
Liquid can not be suitable for hard charcoal cathode and metallic tin cathode.The all charging curves of head of comparative example are shown in Fig. 2.
Embodiment two：
It is identical as one technique of embodiment, the difference is that the ratio of positive plate is positive electrode：Conductive agent：Binder=
80%：10%：10%.Charge and discharge are same as Example 1 with security test.Circulation volume conservation rate still has 75% within 1000 weeks.
Embodiment three：
It is identical as one technique of embodiment, the difference is that assembling just extremely NaFePO4, cathode TiP2O7Full electricity
Pond.Charge and discharge are same as Example 1 with security test, and circulation volume conservation rate still has 94% within 160 weeks.Sodium-ion battery is permanent
Current cycle figure is shown in Fig. 6.
Example IV：
It is identical as one technique of embodiment, the difference is that assembling just extremely Na2FeP2O7, cathode NaTi2(PO4)3's
Full battery.Charge and discharge are same as Example 1 with security test, first Zhou Rongliang 48mAh g-1, capacity retention ratio is within 20 weeks
99.3%.Sodium-ion battery constant current cycle figure is shown in Fig. 7.
Embodiment five：
Identical as one technique of embodiment, difference is electricity in the trimethyl phosphate that electrolyte used is the NaTFSI containing 1M
Solve liquid.Charge and discharge are same as Example 1 with security test, and 1000 weeks circulation volume conservation rates are 74%.
Embodiment six：
Identical as one technique of embodiment, difference is electrolysis in the triethyl phosphate that electrolyte used is the NaFS containing 1M
Liquid.Charge and discharge are same as Example 1 with security test, and first week discharge capacity is 115mAh g-1。
Embodiment seven：
Identical as one technique of embodiment, difference is electricity in the trimethyl phosphate that electrolyte used is the NaFS containing 1.2M
Solve liquid.Charge and discharge are same as Example 1 with security test, and first week discharge capacity is 117mAh g-1。
Above disclosed is only presently preferred embodiments of the present invention, and the right model of the present invention cannot be limited with this
It encloses, therefore according to equivalent variations made by scope of the present invention patent, still falls within the range of the present invention covered.
Claims (10)
1. a kind of safe full phosphate sodium ion secondary battery, including anode, cathode, diaphragm and electrolyte, it is characterised in that：
Positive active material is NaFePO4、Na3V2(PO4)3、Na2FeP2O7、Na2MnP2O7、Na2CoP2O7、Na7V3(P2O7)4,
Na2FePO4F、Na3V2(PO4)2F3、Na4Fe3(PO4)2(P2O7)、Na4Co3(PO4)2(P2O7) in one kind；Negative electrode active material
For NaTi2(PO4)3, Na2TiCr(PO4)3、NaZr2(PO4)3、Na1.5Fe0.5Ti1.5(PO4)3、TiP2O7In one kind；Described
Electrolyte is non-combustible phosphate or phosphonate species electrolyte containing sodium salt.
2. full phosphate sodium ion secondary battery according to claim 1, it is characterised in that：The anode pole piece is by just
Pole active material, conductive agent and binder are prepared, and the cathode pole piece is by negative electrode active material, conductive agent and bonding
Agent is prepared.
3. full phosphate sodium ion secondary battery according to claim 2, it is characterised in that：Anode pole piece preparation method
For：Positive active material, conductive agent and binder are mixed in proportion, solvent is added and is tuned into slurry, is coated on aluminium foil,
It being dried in vacuum overnight and can be obtained anode pole piece, the mass percent of positive active material, conductive agent and binder is 60~
90%：5~20%：5~20%；
The specific preparation method of cathode pole piece is：Negative electrode active material, conductive agent and binder are mixed in proportion, are added molten
Agent is tuned into slurry, is coated on aluminium foil, is dried in vacuum overnight and can be obtained cathode pole piece, negative electrode active material, conductive agent and viscous
The mass percent for tying agent is 60~90%：5~20%：5~20%.
4. full phosphate sodium ion secondary battery according to claim 1, it is characterised in that：Conductive agent is acetylene black, section
Qin is black, one or more of Super P, and binder is polyvinylidene fluoride, polytetrafluoroethylene (PTFE), sodium carboxymethylcellulose, poly-
One or more of butadiene-styrene rubber, polyacrylic acid, sodium alginate, solvent are one kind in N-Methyl pyrrolidone, water.
5. full phosphate sodium ion secondary battery according to claim 1, it is characterised in that：Phosphate or phosphonic acid ester object
The structure of matter is (RO)3P=O or R (RO2) P=O, the lower alkyl groups or halogenated alkyl that R is phenyl or carbon chain lengths are 1-6.
6. full phosphate sodium ion secondary battery according to claim 1, it is characterised in that：Phosphate or phosphonic acid ester object
Matter is triphenyl phosphate, trimethyl phosphate, triethyl phosphate, dimethyl methyl phosphonate, bis- (2,2,2- trifluoroethyls) methyl phosphorus
Acid esters.
7. full phosphate sodium ion secondary battery according to claim 1, it is characterised in that：Sodium salt is sodium perchlorate, six
One or more of sodium fluoro phosphate, double trifluoromethanesulfonimide sodium, trifluoromethayl sulfonic acid sodium.
8. full phosphate sodium ion secondary battery according to claim 1, it is characterised in that：The sodium salt a concentration of 0.5
~3 moles every liter.
9. full phosphate sodium ion secondary battery according to claim 1, it is characterised in that：Diaphragm be polyimide film,
Glass fibre membrane, polyacrylonitrile film, polyethylene terephthalate film, polyether-ether-ketone film, one kind in polytetrafluoroethylene film or
Composite membrane.
10. full phosphate sodium ion secondary battery according to claim 1, it is characterised in that：Described is positive and negative highly preferred
It is as follows to combine (anode/cathode)：Na3V2(PO4)3/NaTi2(PO4)3, Na3V2(PO4)3/Na2TiCr(PO4)3、Na3V2(PO4)2F3/NaTi2(PO4)3、Na3V2(PO4)3/Na1.5Fe0.5Ti1.5(PO4)3、Na2FeP2O7//NaTi2(PO4)3、NaFePO4/
TiP2O7。
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109921021A (en) * | 2019-03-13 | 2019-06-21 | 欧格尼材料科技江苏有限公司 | A kind of high potential high capacity organic polymer positive electrode and its preparation method and application |
| CN112510198A (en) * | 2020-12-16 | 2021-03-16 | 武汉大学 | Positive electrode active material, aqueous solution sodium ion battery and electronic device |
| CN113437276A (en) * | 2021-06-26 | 2021-09-24 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, electrochemical device, and electronic device |
| CN113437275A (en) * | 2021-06-26 | 2021-09-24 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, electrochemical device, and electronic device |
| CN113506912A (en) * | 2021-06-17 | 2021-10-15 | 山东玉皇新能源科技有限公司 | Sodium ion battery electrolyte and application thereof in sodium ion battery |
| CN114243005A (en) * | 2021-12-18 | 2022-03-25 | 复旦大学 | Wide-temperature-range sodium ion battery based on iron-based polyanionic anode and carbon-based cathode |
| CN114792843A (en) * | 2022-03-02 | 2022-07-26 | 温州大学碳中和技术创新研究院 | Sodium ion battery high-voltage electrolyte suitable for high-voltage positive electrode material, and preparation method and application thereof |
| CN115472784A (en) * | 2022-08-16 | 2022-12-13 | 北京航空航天大学 | Na 3 Ti 2 (PO 4 ) 3 Preparation method of positive electrode and application of positive electrode in sodium ion battery |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109921021A (en) * | 2019-03-13 | 2019-06-21 | 欧格尼材料科技江苏有限公司 | A kind of high potential high capacity organic polymer positive electrode and its preparation method and application |
| CN112510198A (en) * | 2020-12-16 | 2021-03-16 | 武汉大学 | Positive electrode active material, aqueous solution sodium ion battery and electronic device |
| CN112510198B (en) * | 2020-12-16 | 2022-06-17 | 武汉大学 | Positive electrode active material, aqueous solution sodium ion battery and electronic device |
| CN113506912A (en) * | 2021-06-17 | 2021-10-15 | 山东玉皇新能源科技有限公司 | Sodium ion battery electrolyte and application thereof in sodium ion battery |
| CN113437276A (en) * | 2021-06-26 | 2021-09-24 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, electrochemical device, and electronic device |
| CN113437275A (en) * | 2021-06-26 | 2021-09-24 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, electrochemical device, and electronic device |
| WO2022267550A1 (en) * | 2021-06-26 | 2022-12-29 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, electrochemical apparatus and electronic device |
| CN114243005A (en) * | 2021-12-18 | 2022-03-25 | 复旦大学 | Wide-temperature-range sodium ion battery based on iron-based polyanionic anode and carbon-based cathode |
| CN114792843A (en) * | 2022-03-02 | 2022-07-26 | 温州大学碳中和技术创新研究院 | Sodium ion battery high-voltage electrolyte suitable for high-voltage positive electrode material, and preparation method and application thereof |
| CN115472784A (en) * | 2022-08-16 | 2022-12-13 | 北京航空航天大学 | Na 3 Ti 2 (PO 4 ) 3 Preparation method of positive electrode and application of positive electrode in sodium ion battery |
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