CN109546134A - The negative electrode material and sodium-ion battery a kind of sodium-ion battery cathode pre- sodium modification method and obtained - Google Patents
The negative electrode material and sodium-ion battery a kind of sodium-ion battery cathode pre- sodium modification method and obtained Download PDFInfo
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- CN109546134A CN109546134A CN201811513254.8A CN201811513254A CN109546134A CN 109546134 A CN109546134 A CN 109546134A CN 201811513254 A CN201811513254 A CN 201811513254A CN 109546134 A CN109546134 A CN 109546134A
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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
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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
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The present invention provides the negative electrode materials and sodium-ion battery a kind of sodium-ion battery cathode pre- sodium modification method and obtain.Anode material of lithium-ion battery is reacted with aryl sodium solution, wherein aryl sodium reagent is conjugated polycyclic aromatic radical sodium compound.Irreversible capacity present in the first all discharge processes of negative electrode material can be eliminated, all coulombic efficiencies of head of cathode are greatly improved.This method can be carried out in room temperature, and the reaction time is short, and simple process, reaction depth is controllable, high safety, is easy to industrialize.Meanwhile the cathode handled through pre- sodium and storage sodium anode match the sodium ion full battery of assembling, energy density and cyclical stability are also substantially improved, so that the functionization for high-energy density sode cell system develops and provides possibility.
Description
Technical field
The present invention relates to a kind of methods of pre- sodium of sodium-ion battery cathode, and obtained negative electrode material and sodium ion electricity
Pond belongs to new energy field.
Background technique
Extensive storage is one of the critical issue of current new energy technology development.Either renewable new energy (such as light
Electricity and wind-powered electricity generation) efficient utilization, or the following clean traffic based on electric vehicle is required to the extensive storage of Cheap highly effective
As technical support.In existing electrochemical energy storage mode, lithium ion battery is with its superior chemical property and by pass
Note, but can the resource reserve of lithium support extensive stored energy application on the earth, be still controversial problem.Sodium-ion battery
Because its sodium is resourceful, low in cost, it is considered to be the ideal alternative solution of energy-storage battery.
Sodium-ion battery commercial applications depend primarily on the development of positive and negative pole material, and wherein negative electrode material is crucial composition
Part.Currently, the research of storage sodium negative electrode material is concentrated mainly on carbon-based material, metal simple-substance or alloy, metal oxide, metal
Sulfide, elemental phosphorous and its compound etc..These materials storage sodium capacity all with higher, long circulation life and high rate performance;
But since its embedding sodium current potential is relatively negative, charge and discharge process becomes non-after easily causing electrolyte decomposition or part sodium ion to be embedded in cathode
Active sodium causes its first all coulombic efficiency mostly lower (60%-85%), this has seriously affected its application in full battery.
For example, document J.Electrochem.Soc., researcher using sucrose as raw material is prepared for hard carbon to store up sodium negative in 2000,147,1271
Pole, reversible storage sodium capacity reaches 300mAh/g, but due to the large specific surface area of carbon material, surface defect is more, and first week efficiency is only
Have 70%.Document Chem.Commun., researcher reports a kind of Sb/C nano-complex, reversible capacity in 2012,48,7070
Up to 610mAh/g, first week efficiency is 83%.Document Nano Lett., Qian etc. is prepared for using ball-milling method in 2014,14,1865
Sn4P3/ C compound, reversible capacity is up to 820mAh/g, but first all efficiency only has 80%.When these negative electrode materials and anode carry out
Matching assembling full battery when, due to negative electrode material for the first time cycle consumption sodium ion need by anode provide, and anode sodium from
Son is limited and is tightly controlled in battery design;Therefore all efficiency of head of negative electrode material to all efficiency of the head of full battery and
Its energy density plays the role of vital.The all coulombic efficiencies of head in order to improve storage sodium cathode, researcher is often using drop
Low specific surface area, reduces the methods of surface functional group and adjusting electrolyte component at raising synthesis temperature.Although these method of modifying
To first all coulombic efficiency effects of haveing a certain upgrade, but the index of all efficiency > 95% of the head required by practical cathode is still
It is far apart.
In order to solve the problems, such as that the first all efficiency of existing anode material of lithium-ion battery is relatively low, the present invention provides a kind of cathode
The all efficiency of head of negative electrode material greatly improved, to be high-energy density sode cell system in the method for the pre- sodium of materials chemistry
Practical development provide possibility.
Summary of the invention
In order to solve the problems, such as that the first all efficiency of existing anode material of lithium-ion battery is relatively low, the present invention provides a kind of cathode
The all efficiency of head of negative electrode material greatly improved, to be high-energy density sode cell system in the method for the pre- sodium of materials chemistry
Practical development provide possibility.
Technical solution of the present invention can be realized by following technical measures:
A kind of pre- sodium modification method of sodium-ion battery cathode carries out anode material of lithium-ion battery and aryl sodium solution anti-
It answers, pre- sodium cathode can be obtained in washed drying, and the solute of the aryl sodium solution is conjugated polycyclic aromatic radical sodium, the virtue
The solvent of base sodium solution is non-protonic solvent.
Preferably, the anode material of lithium-ion battery includes negative electrode active material or cathode pole piece, the battery cathode
The mode of material and sodium aryl solution reaction includes: that aryl sodium solution is coated in negative electrode material surface or soaks negative electrode material
Bubble reacts certain time in fragrant sodium solution.The reaction time of the aryl sodium solution and negative electrode material is 1min~48h, excellent
Select 5min-24h.
The cathode pole piece comprises the following components in parts by weight: 70~99 parts of negative electrode active materials, 0.5~10 part of conduction
Agent, 0.5~10 part of bonding agent.The conductive agent is one or more of acetylene black, Ketjen black, Super P or above-mentioned material.
The binder is one or more of PVDF, CMC, PAA or above-mentioned material.
Preferably, the sodium-ion battery negative electrode active material includes: carbon-based material, silicon substrate, tinbase, antimony base, phosphorus base list
The compound of one or more of matter and its compound, metal oxide, metal sulfide, metal phosphide.
The molar ratio of negative electrode active material and sodium in aryl sodium solution is 1:0.01-1000, preferably 1:0.05- when reaction
20。
Preferably, the solute of the aryl sodium solution be biphenyl sodium, it is bipyridyl sodium, naphthalene sodium, anthracene sodium, any one in luxuriant and rich with fragrance sodium
Kind is several.The concentration of solute is 0.001-10mol/L, more preferably 0.05~5mol/L in the aryl sodium solution.
Preferably, the solvent of the aryl sodium solution is ether, glycol dimethyl ether, diethylene glycol dimethyl ether, three second two
Diethylene glycol dimethyl ether, tetraethyleneglycol dimethyl ether, methyl tertiary butyl ether(MTBE), acetonitrile are any one in n,N-Dimethylformamide, dimethyl sulfoxide
Kind is several.
The present invention also provides a kind of pre- sodium negative electrode materials, adopt and are prepared with the aforedescribed process.
The present invention also provides a kind of sodium-ion battery, the negative electrode material of the sodium-ion battery is adopted to be made with the aforedescribed process
Standby obtained pre- sodium negative electrode material, the battery cathode including pre- sodium, sodium-ion battery anode, diaphragm, electrolyte.Its anode
It can be sodium base transition metal oxide (such as cobalt acid sodium, sodium manganate, sodium ferrite), sodium base transition metal phosphate (such as ferric phosphate
Sodium, vanadium phosphate sodium, fluorophosphate vanadium sodium, ferric sodium pyrophosphate etc.), sodium base transition metal cyanogen root compound (such as sodium ferrocyanide, it is general
One or more of Shandong scholar's indigo plant class compound etc.).
Compared with prior art, the invention has the following beneficial effects:
The aryl sodium reagent that the present invention selects property mild carries out pre- sodium processing to anode material of lithium-ion battery, and
The method is normal-temperature reaction, and the reaction time is short, simple process, high safety, is easy to industrialize.Meanwhile with the cathode of pre- sodium with
Anode matches, and will also promote the raising of the energy density and cyclical stability of full battery, promotes the industrialization of sodium-ion battery
Process.
Detailed description of the invention
The present invention will be further described with reference to the accompanying drawings, but the embodiment in attached drawing is not constituted to any limit of the invention
System.
Fig. 1 is all charging and discharging curve figures of head before and after the pre- sodium of hard carbon electrode of embodiment 1;
Fig. 2 is the hard carbon electrode long-term cycle stability figure of the pre- sodium processing of embodiment 1;
Fig. 3 is all charging and discharging curve figures of head before and after the pre- sodium of Sb/C cathode of embodiment 2;
Fig. 4 is all charging and discharging curve figures of the head of the pre- sodium of Sn4P3/C cathode of embodiment 3 before and after the processing.
Specific embodiment
Explanation technical solution of the present invention is further described with reference to embodiments, but these embodiments are not meant as limiting
Protection scope of the present invention processed.Related experimental material can be purchased unless otherwise instructed by market in the following embodiments
The preparation method for obtaining or passing through this field routine obtains.
Embodiment 1
Equimolar biphenyl and metallic sodium are mixed, are dissolved in glycol dinitrate ether solvents, the connection of 0.25mol/L is made
Benzene sodium solution.10mL biphenyl sodium solution is taken, 1g hard carbon powder is added, reacts 10min under inert atmosphere protection.Product is through taking out
Filter, washing are drying to obtain the hard carbon material of pre- sodium, prepare cathode pole piece using the hard carbon material as negative electrode active material.Fig. 1 pairs
Charging and discharging curve more all than the head for the cathode pole piece that hard carbon material before and after pre- sodium is active material.As seen from the figure, untreated
The all efficiency of the head of hard carbon cathode is only 60.7%, and first all efficiency is obviously improved to 95.8% after the processing of pre- sodium;First week simultaneously
Reversible capacity is increased slightly from 269mAh/g to 293mAh/g.Fig. 2 is the long-term cycle stability of hard carbon cathode after pre- sodium, is held
Measuring conservation rate is 73.21%, shows that pre- sodium processing does not influence the cyclical stability of electrode material.
Embodiment 2
Equimolar naphthalene and metallic sodium are mixed, are dissolved in diethylene glycol dimethyl ether solvent, the naphthalene of 0.5mol/L is made
Sodium solution.Sb/C compound electric pole piece is immersed in the sodium naphthalene solution and reacts 30min, washs drying after the reaction was completed, can be obtained
The Sb/C negative electrode tab of pre- sodium processing.Fig. 3 compared all charging and discharging curves of head of pre- sodium Sb/C cathode before and after the processing.From figure
As it can be seen that all efficiency of head of untreated Sb/C cathode is only 85.23%, first all improved efficiencies are extremely after the processing of pre- sodium
97.5%, and the reversible capacity of material is kept approximately constant.
Embodiment 3
Equimolar luxuriant and rich with fragrance and metallic sodium is mixed, is dissolved in tetraethyleneglycol dimethyl ether solvent, the phenanthrene of 0.1mol/L is made
Sodium solution.By freshly prepared luxuriant and rich with fragrance sodium solution even application in Sn4P3/ C electrode slice surface stands 20min, washes after the reaction was completed
Drying is washed, the Sn of pre- sodium processing can be obtained4P3/ C electrode.Fig. 4 compared Sn before and after pre- sodium4P3The charge and discharge of/C-material are bent
Line.It can be seen that untreated Sn4P3The all charge/discharge capacities of the head of/C-material are 846.2/1055.2mAh/g, first week efficiency
Only 80.2%.After the processing of pre- sodium, first week dischargeable capacity is 851.7/878.7mAh/g, and coulombic efficiency is promoted to
96.9%, the pre- sodium processing in surface eliminates first all irreversible capacities, improves the coulombic efficiency of material.
Embodiment 4
Cathode made above and common storage sodium anode are matched, sodium ion full battery is assembled into, assesses pre- sodium
The influence of positive and negative anodes matching of the processing to full battery, capacity utilization, coulombic efficiency and cyclical stability etc..Table 1 is several
The chemical property of full battery compares.As seen from the table, the pole piece of pre- sodium processing effectively improves the capacity benefit of full battery
With rate and first all efficiency, and long-term cycle stability has also obtained a degree of promotion.
The sodium ion full battery performance comparison that table 1. is assembled using the cathode of pre- sodium processing
In conclusion the method significant effect of pre- sodium is carried out to sodium-ion battery cathode using aryl sodium reagent, it is easy
It is easy, it is highly-safe, and the chemical property of material itself is not influenced.After being matched with the electrode of the pre- sodium of the method into full battery,
First all high-efficient, higher full batteries of energy density can be obtained, there is wide Research Prospects and application value.
Embodiment described above is preferred embodiment of the invention, not does any type of limitation to the present invention,
There are also other variants and remodeling under the premise of without departing from technical solution documented by claim.
Claims (10)
1. a kind of pre- sodium modification method of sodium-ion battery cathode, it is characterised in that: anode material of lithium-ion battery is molten with sodium aryl
Liquid is reacted, and pre- sodium negative electrode material can be obtained in washed drying, and the solute of the aryl sodium solution is conjugated polycyclic virtue
Perfume base sodium, the solvent of the aryl sodium solution are non-protonic solvent.
2. the pre- sodium modification method of sodium-ion battery cathode according to claim 1, it is characterised in that: the sodium-ion battery is negative
Pole material includes negative electrode active material or cathode pole piece, and the mode of the cell negative electrode material and sodium aryl solution reaction includes:
Aryl sodium solution is coated in negative electrode material surface or negative electrode material is immersed in fragrant sodium solution and is reacted.
3. the pre- sodium modification method of sodium-ion battery cathode according to claim 2, it is characterised in that: the cathode pole piece includes
The component of following parts by weight: 70~99 parts of negative electrode active materials, 0.5~10 part of conductive agent, 0.5~10 part of bonding agent.
4. the pre- sodium modification method of sodium-ion battery cathode according to claim 2 or 3, it is characterised in that: the negative electrode active
Material includes: carbon-based material, silicon substrate, tinbase, antimony base, phosphorus base simple substance and its compound, metal oxide, metal sulfide, gold
Belong to the compound of one or more of phosphide.
5. the pre- sodium modification method of sodium-ion battery cathode according to claim 1, it is characterised in that: in the aryl sodium solution
The concentration of solute is 0.05~5mol/L.
6. the pre- sodium modification method of sodium-ion battery cathode according to claim 1, it is characterised in that: the aryl sodium solution
Solute is biphenyl sodium, bipyridyl sodium, naphthalene sodium, anthracene sodium, any one or a few in luxuriant and rich with fragrance sodium.
7. the pre- sodium modification method of sodium-ion battery cathode according to claim 1, it is characterised in that: the aryl sodium solution
Solvent is ether, glycol dimethyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethyleneglycol dimethyl ether, methyl- tert fourth
Base ether, acetonitrile, any one or a few in n,N-Dimethylformamide, dimethyl sulfoxide.
8. the pre- sodium modification method of sodium-ion battery cathode according to claim 1, it is characterised in that: the aryl sodium solution with
The reaction time of anode material of lithium-ion battery is 1min~48h.
9. a kind of pre- sodium negative electrode material, which is characterized in that be prepared into using method described in claim 1 to 8 any one
It arrives.
10. a kind of sodium-ion battery, which is characterized in that the negative electrode material of the sodium-ion battery is appointed using in claim 1 to 8
The pre- sodium negative electrode material that method described in meaning one is prepared.
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Cited By (8)
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CN110707308A (en) * | 2019-10-23 | 2020-01-17 | 湖南立方新能源科技有限责任公司 | Negative electrode sodium supplement additive, negative electrode material and sodium ion battery |
CN110931754A (en) * | 2019-12-12 | 2020-03-27 | 宁德新能源科技有限公司 | Negative electrode material, preparation method thereof, negative electrode plate and electrochemical device |
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 |
CN112952037A (en) * | 2021-02-25 | 2021-06-11 | 武汉大学 | Pre-sodium-modified sodium ion battery positive electrode and pre-sodium-modification method and application thereof |
CN113113235A (en) * | 2021-04-15 | 2021-07-13 | 中国科学院电工研究所 | Sodium ion capacitor and negative electrode pre-sodium treatment method thereof |
CN113130853A (en) * | 2021-04-19 | 2021-07-16 | 中国科学技术大学 | Modified alkali metal ion battery negative plate, preparation method and application thereof |
CN117254120A (en) * | 2023-11-10 | 2023-12-19 | 中自环保科技股份有限公司 | Sodium ion battery and pre-sodium treatment method thereof |
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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 |
CN110707308A (en) * | 2019-10-23 | 2020-01-17 | 湖南立方新能源科技有限责任公司 | Negative electrode sodium supplement additive, negative electrode material and sodium ion battery |
CN110707308B (en) * | 2019-10-23 | 2022-09-16 | 湖南钠方新能源科技有限责任公司 | Negative electrode sodium supplement additive, negative electrode material and sodium ion battery |
CN110931754A (en) * | 2019-12-12 | 2020-03-27 | 宁德新能源科技有限公司 | Negative electrode material, preparation method thereof, negative electrode plate and electrochemical device |
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 |
CN112635709B (en) * | 2020-12-15 | 2022-06-28 | 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 |
CN112952037A (en) * | 2021-02-25 | 2021-06-11 | 武汉大学 | Pre-sodium-modified sodium ion battery positive electrode and pre-sodium-modification method and application thereof |
CN112952037B (en) * | 2021-02-25 | 2022-11-11 | 深圳珈钠能源科技有限公司 | Pre-sodium-modified sodium ion battery positive electrode and pre-sodium-modification method and application thereof |
CN113113235A (en) * | 2021-04-15 | 2021-07-13 | 中国科学院电工研究所 | Sodium ion capacitor and negative electrode pre-sodium treatment method thereof |
CN113113235B (en) * | 2021-04-15 | 2022-11-15 | 中国科学院电工研究所 | Sodium ion capacitor and negative electrode pre-sodium treatment method thereof |
CN113130853A (en) * | 2021-04-19 | 2021-07-16 | 中国科学技术大学 | Modified alkali metal ion battery negative plate, preparation method and application thereof |
CN117254120A (en) * | 2023-11-10 | 2023-12-19 | 中自环保科技股份有限公司 | Sodium ion battery and pre-sodium treatment method thereof |
CN117254120B (en) * | 2023-11-10 | 2024-02-02 | 中自环保科技股份有限公司 | Sodium ion battery and pre-sodium treatment method thereof |
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