CN107240715A - A kind of easy negative pole processing method for improving the full cell voltage of sodium ion and efficiency - Google Patents
A kind of easy negative pole processing method for improving the full cell voltage of sodium ion and efficiency Download PDFInfo
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- CN107240715A CN107240715A CN201710540148.8A CN201710540148A CN107240715A CN 107240715 A CN107240715 A CN 107240715A CN 201710540148 A CN201710540148 A CN 201710540148A CN 107240715 A CN107240715 A CN 107240715A
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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
- 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
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The present invention relates to a kind of easy negative pole processing method and product for improving the full cell voltage of sodium ion and efficiency, belong to sodium-ion battery technical field, this method is specially：（1）Prepare negative plate：Negative material, conductive agent and bonding agent are added in solvent respectively, the cathode size of dark thick shape is made after grinding, the cathode size is applied on collector, after drying process, negative plate is made；（2）The pre- sodium of negative pole：By the pre- sodium method of excessive cathode contact formula to step（1）In obtained negative plate carry out pre- sodium processing.The negative pole treated by such a method possesses embedding sodium current potential minimum in current all materials reported, so as to lift the voltage of full battery to greatest extent；But also the first circle efficiency of full battery can be effectively improved.Different with the pre- sodium method of electrochemistry delivered before us, this kind of method is easy to operate, and effect is obvious, more commercial value.
Description
Technical field
The invention belongs to sodium-ion battery technical field, and in particular to a kind of processing method of anode material of lithium-ion battery
And product.
Background technology
Current era, with the development and the popularization of mobile electronic device of electric automobile, need of the people to lithium ion battery
The amount of asking is also increasing.Yet with the scarcity of lithium resource, following application of lithium ion battery and development is caused to be faced with huge
The problem of., will continuous rise in the price of following lithium ion battery from referring now to.So under this serious situation,
The developing low-cost and abundanter sodium-ion battery of resource is significant.
The problem of being faced with heavy in sodium-ion battery commercialization, the research of sodium-ion battery positive material at present is
Through substantially tending to be ripe.Although the positive electrode of metal oxide-type is with good specific capacity, multi-platform operating voltage,
But be due to sodium ion radius ratio lithium ion it is big so that this kind of material lattice knot during the embedded abjection of sodium ion
Structure is easier avalanche so that the cyclical stability of this kind of material is generally less desirable.By contrast, polyanion class positive pole material
Material possesses more stable crystal structure so that its cyclical stability will generally be better than the material of metal oxide-type, along with poly-
The inductive effect that anion is brought is present so that the voltage of this kind of material is generally higher, and this also compensate for a certain extent
The problem of sodium-ion battery voltage is relatively low.At present, the greatest problem faced during sodium ion industrialization will count negative
The selection of pole, this negative pole must simultaneously meet low embedding sodium current potential, good cyclical stability and high first circle efficiency etc.
A variety of conditions.Current research of the people to negative pole is concentrated mainly in two major classes, and one kind is metal oxide, and one kind is carbon materials
Material.But metal oxide involves great expense, and theoretical capacity is not generally very high, and the circulation of most metal oxide is steady
Qualitative is not highly desirable.In addition, the embedding sodium current potential of metal oxide is also universal too high, and this causes to have used metal oxidation
Thing can be reduced as the full cell voltage of negative pole.In contrast to this, carbon material is cheap, and theoretical capacity is higher, embedding sodium
Current potential is lower, undoubtedly optimal negative material in sodium-ion battery commercialization, yet with carbon material in first circle discharge and recharge
During can form very thick SEI films, in this full battery the formation consumption of this SEI film be sodium in positive electrode from
Son, so the capacity of full battery can be made to have obvious loss after first circle.Further, since the characteristic of hard carbon in itself, causes
The embedding sodium platform of hard carbon is delayed, and the voltage for making full battery that the gentle slope voltage before embedding sodium current potential can be serious declines, so that
The full battery energy density prepared declines.So, solving research of the two problems to the full battery of sodium-ion battery has great meaning
Justice.
We organize before by the embedding sodium method of electrochemistry it is relatively good solve this problem, but be due to electrochemical process operation
Complexity, experiment condition is strict, so being not to be well suited for commodity production.Then we further study, and have found one kind and connect
The pre- sodium method of touch.Compared with electrochemical process, the method is easier, condition requires also strict not as electrochemical process, than
Electrochemical process has more commercial significance.
The content of the invention
In view of this, it is an object of the invention to：（1）A kind of letter for improving the full cell voltage of sodium ion and efficiency is provided
Just negative pole processing method；（2）A kind of sodium-ion battery negative plate is provided；（3）There is provided a kind of sodium ion full battery.
To reach above-mentioned purpose, the present invention provides following technical scheme：
1st, a kind of easy negative pole processing method for improving the full cell voltage of sodium ion and efficiency, comprises the following steps：
（1）Prepare cathode pole piece：Negative material, conductive agent and bonding agent are added in solvent respectively, black is made after grinding and glues
The cathode size of thick shape, the cathode size is applied on collector, after drying process, and negative plate is made；
（2）The pre- sodium of negative pole：Using contact method to step（1）In obtained negative plate carry out pre- sodium processing.
Further, step（1）In, the mass ratio of the negative material, conductive agent and bonding agent is 8：1：1.
Further, step（1）In, the negative material is hard carbon.
Further, step（1）In, the conductive agent is the one or more in acetylene black, conductive carbon black or Ketjen black；Institute
It is the one or more in Kynoar, carboxymethyl cellulose, polystyrenebutadienes copolymer, the solvent to state bonding agent
For 1-Methyl-2-Pyrrolidone, the collector is aluminium foil.
Further, step（1）In, the drying process is to be dried in vacuo 12 ~ 24 hours at 60 ~ 120 DEG C.
Further, step（2）In, the contact method is specially：By step（1）In obtained negative plate in inert gas ring
It is put under border in suitable container, appropriate electrolyte is added in a reservoir, metallic sodium piece is pressed against on negative plate, applies 25
kg/cm2~50 kg/cm2It is stood to 5 ~ 30 minutes in an inert atmosphere after pressure, pre- sodium removes negative plate after terminating,
Obtain the negative plate that pre- sodium is finished.
2nd, born as made from the easy negative pole processing method of described a kind of full cell voltage of raising sodium ion and efficiency
Pole piece.
3rd, the full battery prepared by described negative plate.
Further, the mass ratio of negative material and positive electrode in the full battery is 1 in the negative plate:1~4:1.
Further, positive electrode is Na in the full battery3V2O2(PO4)2F/rGO.Specifically synthetic method is：40 milligrams
Graphene oxide（GO）Ultrasonic disperse is in 50 milliliters of N, N- dimethyl amides（DMF）In.It is dissolved in 10 ml deionized waters
In 0.001 mole and 0.0015 mole of ammonium metavanadate and sodium fluoride be slowly dropped into above-mentioned system.Then 10 are dissolved in
0.001 mole of diammonium hydrogen phosphate in ml deionized water is slowly dropped into above-mentioned system.By above-mentioned solution at 80 degrees celsius
In four hours of stirring in water bath, the reactor for being then transferred to 100 milliliters, 180 degrees Celsius are reacted 12 hours.Finally by taking out
Filter, is dried to obtain final product.
The beneficial effects of the present invention are：The invention provides a kind of letter for improving the full cell voltage of sodium ion and efficiency
Just negative pole processing method and product, this method are the pre- sodium method of excessive cathode contact formula, and current institute can be obtained by the method
There is embedding sodium current potential minimum in known negative material, so as to lift the voltage of full battery to greatest extent；Further, by such a
Method can also significantly improve full battery first circle efficiency.Finally, compared with electrochemical process, such a method is easier, more business
Industry is worth.
Brief description of the drawings
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, the present invention provides drawings described below and carried out
Explanation：
Fig. 1 is the constant current charge-discharge diagram of positive electrode used（It is left）With cyclical stability figure（It is right）；
Fig. 2 is the constant current charge-discharge diagram of negative material used（It is left）With cyclical stability figure（It is right）；
Fig. 3 is the principle explanatory diagram of the full cell voltage of lifting of the pre- sodium method of excessive cathode contact formula；
Fig. 4 is the full battery constant current charging-discharging figure prepared by this method（It is left）With cyclical stability figure（It is right）；
Fig. 5 is the full battery constant current charging-discharging figure prepared not over this method（It is left）With cyclical stability figure（It is right）.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.
Embodiment 1
With Na3V2O2(PO4)2F/RGO is positive pole, the full battery production method by negative pole of hard carbon.
（1）The making of cathode pole piece：The negative material and conductive agent and binding agent of 2 times of positive electrode will be in excess in by matter
Amount compares 8:1:After 1 ratio mixing, 1-Methyl-2-Pyrrolidone is added（NMP）In, grind 20 minutes, obtain in agate mortar
To the cathode size of dark thick.Cathode size is taken uniformly to be applied to scraper on aluminium foil, 120 DEG C are dried in vacuo 12 hours.
Then aluminium foil is cut into a diameter of 19 mm circle with tablet press machine, negative plate is produced.
（2）The pre- sodium of negative pole：By step（1）Middle gained negative plate is put into suitable container in an inert atmosphere,
Appropriate electrolyte is added in a reservoir, metallic sodium piece is pressed against on negative plate, applies 50 kg/cm2By it lazy after pressure
30 min are stood under property gaseous environment.Pre- sodium removes electrode after terminating, and obtains the negative plate that pre- sodium is finished.
（3）Full battery assembling：By positive electrode, barrier film and step（2）In the negative material that finishes of pre- sodium carry out knob
The assembling of battery is detained, the button cell model used is CR2032, and barrier film model whatman GF/D, electrolyte is 1 mol/
L NaClO4Solution（Solvent is ethylene carbonate and dimethyl carbonate by volume 1:The mixed liquor of 1 composition）.Assembling is finished
Afterwards, by battery removal glove box, tested after standing 6h at 30 DEG C in Land test systems.
Embodiment result is shown in Fig. 3.
Embodiment 2
The not no full battery production method Jing Guo pre- sodium
Preparation method is unique the difference is that not passing through step with reference to embodiment 1（2）Pre- sodium.
Embodiment result is shown in Fig. 5.
Fig. 1 is positive electrode Na used3V2O2(PO4)2F/rGO constant current charge-discharge diagram and cyclical stability figure, can by Fig. 1
Know, the voltage platform of used positive electrode is 3.7 V and and the positive electrode possesses good stable circulation performance.
Fig. 2 is the constant current charge-discharge diagram and cyclical stability figure of negative material hard carbon used, as shown in Figure 2, hard carbon material
Capacity be 300 MAhs/g or so, its amount of capacity fully meets the demand as the full cell negative electrode material of sodium ion, but
It is that hard carbon material possesses two voltage platforms, wherein 0 ~ 0.1 V voltage platform is quite gentle, is very suitable for doing the negative of full battery
Pole, and 0.1 ~ 1 V voltage platform is high and precipitous, can cause the platform of full battery reduces and becomes precipitous.
Fig. 3 is the principle explanation to this method, because the negative pole used is excessive so that the capacity of negative pole is far longer than
Positive electrode, so as to will not rise the voltage of negative material when causing the sodium ion in positive electrode to enter negative material
To 0.1 more than V, and the voltage of full battery subtracts the voltage of negative material for the voltage of positive electrode, so as to reach that lifting is complete
The purpose of cell voltage.As can be known from Figure, used after the method, the voltage of full battery compared with half-cell almost not under
Drop.
Fig. 4 be by a process for preparing full battery constant current charge-discharge diagram and cyclical stability figure, as shown in Figure 4,
The full cell voltage platform stable prepared by this method, cycle performance is outstanding.
Fig. 5 is constant current charge-discharge diagram and cyclical stability figure not by the full battery prepared by this method, by Fig. 5
Understand, it is big in positive electrode in first circle charging process not by the treated negative pole of the pre- sodium method of excessive cathode contact formula
The sodium ion of amount can form SEI films and solid solution sodium, cause the loss of full battery capacity.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
Cross above preferred embodiment the present invention is described in detail, it is to be understood by those skilled in the art that can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (10)
1. a kind of easy negative pole processing method for improving the full cell voltage of sodium ion and efficiency, it is characterised in that including as follows
Step：
（1）Prepare negative plate：Negative material, conductive agent and bonding agent are added in solvent respectively, dark thick is made after grinding
The cathode size of shape, cathode size is applied on collector, after drying process, and negative plate is made；
（2）The pre- sodium of negative pole：Using contact method to step（1）In obtained negative plate carry out pre- sodium processing.
2. a kind of easy negative pole processing method for improving the full cell voltage of sodium ion and efficiency as claimed in claim 1, its
It is characterised by, the step（1）In negative material be hard carbon；The conductive agent is in acetylene black, conductive carbon black or Ketjen black
One or more；The step（1）In bonding agent be Kynoar, carboxymethyl cellulose or polystyrenebutadienes it is common
One or more in polymers；The step（1）In solvent be 1-Methyl-2-Pyrrolidone；The step（1）In afflux
Body is aluminium foil.
3. a kind of easy negative pole processing method for improving the full cell voltage of sodium ion and efficiency as claimed in claim 1, its
It is characterised by, the step（1）The mass ratio of middle negative material, conductive agent and bonding agent is 8：1：1.
4. a kind of easy negative pole processing method for improving the full cell voltage of sodium ion and efficiency as claimed in claim 1, its
It is characterised by, the step（1）Middle drying process is to be dried in vacuo 12-24 hours at 60 ~ 120 DEG C.
5. the easy negative pole processing of a kind of full cell voltage of raising sodium ion and efficiency as described in claim any one of 1-4
Method, it is characterised in that the step（2）In contact method be specially：By step（1）In obtained negative plate in inert gas
It is put under environment in suitable container, appropriate electrolyte is added in a reservoir, metallic sodium piece is pressed against on negative plate, is applied
25 kg/cm2~50 kg/cm2It is stood to 5 ~ 30 minutes in an inert atmosphere after pressure, pre- sodium removes negative pole after terminating
Piece, that is, obtain the negative plate that pre- sodium is finished.
6. a kind of easy negative pole processing method for improving the full cell voltage of sodium ion and efficiency as claimed in claim 5, its
It is characterised by, the electrolyte in described electrolyte is the one or more of sodium perchlorate and sodium hexafluoro phosphate；The electrolyte
In solution be ethylene carbonate, dimethyl carbonate, the one or more of makrolon and fluorinated ethylene carbonate；The electrolysis
The concentration of liquid is one mole every liter.
7. handled as a kind of full cell voltage of raising sodium ion described in claim any one of 1-6 and the easy negative pole of efficiency
Negative plate made from method.
8. the full battery prepared as the negative plate described in claim 7.
9. full battery as claimed in claim 8, it is characterised in that positive electrode is to be synthesized by hydro-thermal method in the full battery
Na3V2O2(PO4)2F/rGO, specific synthetic method is：40mg graphene oxides（GO）Ultrasonic disperse is in 50 milliliters of N, N- bis-
Methyl diamides（DMF）In；0.001 mole be dissolved in 10 ml deionized waters and 0.0015 mole of ammonium metavanadate and
Sodium fluoride is slowly dropped into above-mentioned system；Then 0.001 mole of diammonium hydrogen phosphate being dissolved in 10 ml deionized waters
It is slowly dropped into above-mentioned system；By above-mentioned solution four hours of stirring in water bath at 80 degrees celsius, 100 milliliters anti-is then transferred to
Answer in kettle, 180 degrees Celsius are reacted 12 hours；Finally by suction filtration, final product Na is dried to obtain3V2O2(PO4)2F/rGO。
10. full battery as claimed in claim 8, it is characterised in that contained negative material in the negative plate in the full battery
Mass ratio with the positive electrode in the full battery is 1:1~4:1.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108899520A (en) * | 2018-07-05 | 2018-11-27 | 武汉理工大学 | Globe daisy shape Na3V2O2(PO4)2F-GO nanocomposite and its preparation method and application |
| CN109546134A (en) * | 2018-12-11 | 2019-03-29 | 武汉大学 | The negative electrode material and sodium-ion battery a kind of sodium-ion battery cathode pre- sodium modification method and obtained |
| CN110247037A (en) * | 2019-06-11 | 2019-09-17 | 华中科技大学 | A kind of fluorophosphoric acid vanadium oxygen sodium/graphene complex and preparation method and purposes |
| CN110335764A (en) * | 2019-07-30 | 2019-10-15 | 中南大学 | A kind of pre- sodium modification method for efficiently constructing sodium ion capacitor |
| CN111224071A (en) * | 2018-11-27 | 2020-06-02 | 北京卫蓝新能源科技有限公司 | Preparation method and application of electrode with high cycle efficiency |
| WO2020174496A1 (en) * | 2019-02-28 | 2020-09-03 | Kpit Technologies Limited | A high-power density sodium-ion battery |
| CN111762769A (en) * | 2020-05-24 | 2020-10-13 | 同济大学 | Preparation method and application of vanadium sodium oxygen fluorophosphate/graphene composite electrode material |
| CN111952532A (en) * | 2019-05-16 | 2020-11-17 | 同济大学 | Sodium ion secondary battery cathode material subjected to pre-sodium treatment and mechanical pre-sodium treatment method thereof |
| CN112635709A (en) * | 2020-12-15 | 2021-04-09 | 合肥工业大学 | SEI film forming agent for negative electrode of sodium-ion battery, pre-sodium treatment method and sodium-ion battery |
| CN114824175A (en) * | 2022-06-28 | 2022-07-29 | 宝晟(苏州)能源科技有限公司 | Sodium ion battery cathode pre-sodium treatment method for preparing electrode film based on dry method |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108899520A (en) * | 2018-07-05 | 2018-11-27 | 武汉理工大学 | Globe daisy shape Na3V2O2(PO4)2F-GO nanocomposite and its preparation method and application |
| CN108899520B (en) * | 2018-07-05 | 2021-07-27 | 武汉理工大学 | Globose Na3V2O2(PO4)2F-GO nano composite material and preparation method and application thereof |
| CN111224071A (en) * | 2018-11-27 | 2020-06-02 | 北京卫蓝新能源科技有限公司 | Preparation method and application of electrode with high cycle efficiency |
| CN111224071B (en) * | 2018-11-27 | 2022-07-12 | 北京卫蓝新能源科技有限公司 | Preparation method and application of electrode with high cycle efficiency |
| CN109546134A (en) * | 2018-12-11 | 2019-03-29 | 武汉大学 | The negative electrode material and sodium-ion battery a kind of sodium-ion battery cathode pre- sodium modification method and obtained |
| WO2020174496A1 (en) * | 2019-02-28 | 2020-09-03 | Kpit Technologies Limited | A high-power density sodium-ion battery |
| CN111952532B (en) * | 2019-05-16 | 2021-11-09 | 同济大学 | Sodium ion secondary battery cathode material subjected to pre-sodium treatment and mechanical pre-sodium treatment method thereof |
| CN111952532A (en) * | 2019-05-16 | 2020-11-17 | 同济大学 | Sodium ion secondary battery cathode material subjected to pre-sodium treatment and mechanical pre-sodium treatment method thereof |
| CN110247037A (en) * | 2019-06-11 | 2019-09-17 | 华中科技大学 | A kind of fluorophosphoric acid vanadium oxygen sodium/graphene complex and preparation method and purposes |
| CN110247037B (en) * | 2019-06-11 | 2021-01-01 | 华中科技大学 | Preparation method and application of sodium vanadium oxygen fluorophosphate/graphene compound |
| CN110335764A (en) * | 2019-07-30 | 2019-10-15 | 中南大学 | A kind of pre- sodium modification method for efficiently constructing sodium ion capacitor |
| CN111762769A (en) * | 2020-05-24 | 2020-10-13 | 同济大学 | Preparation method and application of vanadium sodium oxygen fluorophosphate/graphene composite electrode material |
| CN112635709A (en) * | 2020-12-15 | 2021-04-09 | 合肥工业大学 | SEI film forming agent for negative electrode of sodium-ion battery, pre-sodium treatment method and sodium-ion battery |
| CN114824175A (en) * | 2022-06-28 | 2022-07-29 | 宝晟(苏州)能源科技有限公司 | Sodium ion battery cathode pre-sodium treatment method for preparing electrode film based on dry method |
| WO2024001591A1 (en) * | 2022-06-28 | 2024-01-04 | 宝晟(苏州)能源科技有限公司 | Sodium-ion battery negative electrode sodium-pre-modification method for preparing electrode film based on dry method |
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