CN110233264A - A kind of sodium-ion battery positive material and preparation method thereof of stratiform sulfoselenide as high rate capability - Google Patents
A kind of sodium-ion battery positive material and preparation method thereof of stratiform sulfoselenide as high rate capability Download PDFInfo
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- CN110233264A CN110233264A CN201910551995.3A CN201910551995A CN110233264A CN 110233264 A CN110233264 A CN 110233264A CN 201910551995 A CN201910551995 A CN 201910551995A CN 110233264 A CN110233264 A CN 110233264A
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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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
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/362—Composites
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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
- H01M4/581—Chalcogenides or intercalation compounds thereof
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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
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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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Abstract
The invention belongs to electrochemical power sources and field of energy source materials, and in particular to a kind of sodium-ion battery positive material and preparation method thereof of stratiform sulfoselenide as high rate capability.The material includes transition metal Cr and nonmetallic S and Se, molecular formula NaCrS simultaneouslyxSe2‑x, 2 > x > 0.Preparation method is by the way that by the vulcanized sodium of stoichiometric ratio, chromium, sulphur, selenium is uniformly mixed, and then the pyroreaction under argon gas stream obtains for tabletting.Material provided by the present invention has fabulous fast charging and discharging high rate performance as sodium-ion battery positive material, and preparation method economy is convenient.Sodium-ion battery and related electronic devices applied to high power density have good prospect.
Description
Technical field
The invention belongs to electrochemical power sources and field of energy source materials, and in particular to a kind of stratiform sulfoselenide is as high magnification
Sodium-ion battery positive material of performance and preparation method thereof.
Background technique
A kind of secondary chemical sources of electric energy of the lithium ion battery as high-energy, has been widely used in various electronic products.
However, it is rare due to lithium resource, hidden danger is caused safely to future source of energy.And sodium resource price is cheap, on earth very
Abundant (content be approximately lithium 12500 times), and since sodium and lithium belong to the first main group, physicochemical properties are similar, thus sodium from
There are sub- battery very big potentiality to substitute lithium ion battery.
Sodium-ion battery positive material is to limit the principal element of battery capacity and various performances.The sodium ion studied at present
Cell positive material is mostly the structure for transplanting anode material for lithium-ion batteries, and lithium ion substitution is made sodium ion.Compared to lithium, by
In the bigger radius of sodium-ion battery, so that it is more difficult compared to lithium ion mobility, and sodium ion migration is to overall structure
Frame influence it is very big.The high rate performance of current existing some sodium-ion battery positive materials (especially layered oxide) is all
It is poor.And it is many be directed to improve its high rate performance researchs be mostly carbon coating is carried out at composite material by manufacture, or
Special pattern and nano material are prepared to realize, cost is high among these, with practical application wide apart.And this patent is created
It selects to the property made the chalcogenide compound with more big frame to improve Na ~+Mobility, and is substantially increased due to joined selenium
Electron conduction.The NaCrS being prepared in this patentxSe2-xWith fabulous fast charge it is fast put high rate performance.
Summary of the invention
A kind of sodium-ion battery positive material the object of the present invention is to provide stratiform sulfoselenide as high rate capability
And preparation method thereof.
A kind of sodium-ion battery positive material of the stratiform sulfoselenide proposed by the present invention as high rate capability, it is described just
Pole material includes transition metal Cr and nonmetallic S and Se simultaneously, is a kind of sulfoselenide of stratiform, and molecular formula is
NaCrSxSe2-x, 2 > x > 0.Sulphur system lamellar compound has bigger cell parameter relative to layered oxide, is conducive to improve
Na ~+Mobility, and the addition of selenium is then conducive to improve electron conduction.In addition, not having such layer also in related fields at present
The report of the sulfoselenide of shape and openly.
In the present invention, the positive electrode is powder, the second particle group as made of the primary particle of sheet and its aggregation
At, and its primary particle is thickness 1-3 microns, the laminated structure that 3-10 microns of size.The piece of this powdery in solid phase preparation
The step of sprills are readily available, and need not move through other or reprocessing can reach.The specific size of particle
Also the ratio with S and Se, temperature-time of heating etc. are related for pattern.
A kind of preparation of sodium-ion battery positive material of the stratiform sulfoselenide proposed by the present invention as high rate capability
Method, by the vulcanized sodium of stoichiometric ratio, chromium, sulphur and selenium mix (molar ratio of vulcanized sodium, chromium, sulphur and selenium total amount be 1:2:3,
Sulphur selenium ratio is any), tabletting, and the product after tabletting is put into argon gas stream and carries out heating reaction, obtain the sodium ion electricity
Pond positive electrode.Solid phase reaction method facilitates economy, can also be produced on a large scale.Wherein vulcanized sodium due to its price compared with
It is expensive, sodium carbonate inexpensively can be used in actual production, carbon, reaction in-situ generates at high temperature than mixing for sulphur metering.
In the present invention, the temperature for heating reaction is 600-1500 DEG C, and heating time is 2-24 hours.
A kind of stratiform sulfoselenide proposed by the present invention as high rate capability sodium-ion battery positive material in anode
Application in material composite, the positive electrode compound include sodium-ion battery positive material, also contain conductive agent and glue
Agent is tied, specifically: conductive agent and binder are added into sodium-ion battery positive material, then add solvent (NMP) slurrying, smear
It is dry in blocks in conductive substrates, or conductive agent and binder are added into sodium-ion battery positive material, smear is in conduction
It is directly dry-mixed tabletted in substrate.
In the present invention, the conductive agent is SPUER Li, S-O, KS-6, KS-15, SFG-6, SFG-15,350G, acetylene black
(AB), one of Ketjen black (KB), gas-phase growth of carbon fibre (VGCF) or carbon nanotube (CNT) or in which several.
In the present invention, the binder is polyvinyl alcohol (PVA), polyvinylidene fluoride (PVDF), polytetrafluoroethylene (PTFE)
(PTFE) or one of sodium cellulose glycolate (CMC) etc. or several.
In the present invention, the drying condition be vacuum under or atmospheric conditions, 50-150 DEG C of drying temperature, drying time 2-
24 hours.
In the present invention, the conductive substrates are one of copper foil, aluminium foil or stainless steel etc. or several.
A kind of stratiform sulfoselenide proposed by the present invention as high rate capability sodium-ion battery positive material sodium from
Application in sub- battery, the sodium-ion battery, including as cathode metallic sodium or hard carbon material compound, diaphragm have
Machine electrolyte and as anode sodium-ion battery positive material.
A kind of sodium-ion battery positive material proposed by the present invention is preparing the application in energy energy storage device.Described one
Kind sodium-ion battery, including the metallic sodium or hard carbon material compound as cathode, diaphragm, organic electrolyte and as anode
Positive electrode.
In the present invention, the organic electrolyte is carbonic ester electrolyte, and concentration 0.1-3mol/L, molten described dose is selected from carbon
Dimethyl phthalate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC), ethylene carbonate (EC), propene carbonate (PC) and
One or more of fluoro ethylene carbonate (FEC).Solute is selected from sodium hexafluoro phosphate (NaPF6), sodium perchlorate (NaClO4) or
One of two (trimethyl fluoride sulfonyl) imines sodium (NaTFSI) are a variety of.
The beneficial effects of the present invention are: material provided by the present invention has pole as sodium-ion battery positive material
Good fast charging and discharging high rate performance, and preparation method economy is convenient.Sodium-ion battery and correlation applied to high power density
Electronic device has good prospect.
Detailed description of the invention
Fig. 1 is the NaCrS of three kinds of different proportions in present invention specific implementationxSe2-xX-ray powder diffraction figure.
Fig. 2 is the SEM image of the positive electrode NaCrSSe in present invention specific implementation.
Fig. 3 is that the positive electrode in present invention specific implementation is sodium-ion battery obtained by NaCrSSe in different charge and discharges
First circle charging and discharging curve under electric current.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not used to limit
The fixed present invention.
Embodiment 1: the preparation of sodium ion positive electrode
Weigh the vulcanized sodium of stoichiometric ratio, sulphur powder and selenium powder.Carefully grinding is uniform in mortar, then tabletting.By what is pressed
Piece is put into the tube furnace of logical argon gas, and sample reacts 6 hours at 900 DEG C.50 are dropped to tubular type furnace temperature after heating
DEG C product is taken out and uses mortar grinder finely ground.Bottling remain using.Three kinds of different proportions are made in choosing in the present embodiment
NaCrSxSe2-x(x=0.5,1,1.5), is listed as follows:
It is the NaCrS of three kinds of different proportions such as Fig. 1xSe2-xX-ray powder diffraction figure (x=0.5,1,1.5).Available material
Expect well-crystallized.Structure belongs to 3 structure of O ' in stratiform.In addition it can be found that with x increase, cell parameter reduce.
Be NaCrSSe(x=1 obtained such as Fig. 2) SEM image, can clearly identify the sheet of sample obtained
Pattern.
Embodiment 2: the preparation of positive electrode compound
By product made from embodiment 1 and PVDF, Super P is uniformly mixed according to mass ratio 8:1:1, and Solvents N-methyl is added
Pyrrolidones stirring is slurried.Slurry is uniformly coated on aluminium foil.Coated pole piece is put into vacuum drying oven, 120 DEG C of bakings
12 hours.The sequin that the pole piece being baked is cut into 12mm diameter is stand-by.
Embodiment 3: sodium-ion battery assembly
By anode sequin made from embodiment 2 and sodium assembled metal at sodium-ion battery, fibreglass diaphragm, electrolyte are selected
It selects the sodium perchlorate of 1mol/L in the ethylene carbonate and methyl carbonate of volume ratio 1:1, and adds 5% volume fluoro carbonic acid
Vinyl acetate.
Embodiment 4: electrochemical property test
Charge and discharge electrical measurement is carried out under different electric currents to the sodium-ion battery obtained that embodiment 3 is prepared using blue electricity
Examination.
It is the positive electrode in present invention specific implementation is that sodium-ion battery obtained by NaCrSSe is filled in difference such as Fig. 3
First circle charging and discharging curve under discharge current.It can be found that it is every with 138 milliampere hour for the first time under 50 milliamperes every gram of electric current
Gram charging capacity and 137.0 every gram of milliampere hour discharge capacity.The speed for improving charge and discharge, in 4000 milliamperes every gram of electric current
Under, that is, charge or discharge is completed in two minutes, charging capacity for the first time there remains 115.5 every gram of milliampere hour
(charge under 50 milliamperes of every gram of electric currents 83.7%), discharge capacity maintain (the 50 milliamperes of every gram of electric current decentralizations of 64.4 every gram of milliampere hour
The 47.0% of electricity).Its advantage with fabulous high rate performance, especially quick charge.
The contents of the present invention have passed through above preferred embodiment and have been discussed in detail, but are not considered as to the present invention
Limitation.After those skilled in the art have read above content, a variety of modifications and substitutions all will be apparent.This
The protection scope of invention should be limited to the appended claims.
Claims (10)
1. a kind of sodium-ion battery positive material of stratiform sulfoselenide as high rate capability, which is characterized in that the anode
Material includes transition metal Cr and nonmetallic S and Se simultaneously, is a kind of sulfoselenide of stratiform, and molecular formula is
NaCrSxSe2-x, 2 > x > 0.
2. sodium-ion battery positive material according to claim 1, which is characterized in that the positive electrode is powder, by
The composition of second particle made of the primary particle of sheet and its aggregation, and its primary particle is thickness 1-3 microns, size 3-10 is micro-
The laminated structure of rice.
3. a kind of system of sodium-ion battery positive material of stratiform sulfoselenide as described in claim 1 as high rate capability
Preparation Method, which is characterized in that mix the vulcanized sodium of stoichiometric ratio, chromium, sulphur and selenium, vulcanized sodium, chromium, sulphur and selenium total amount are rubbed
, than being 1:2:3, sulphur selenium ratio is any, tabletting, and the product after tabletting is put into argon gas stream and carries out heating reaction, obtains institute for you
State sodium-ion battery positive material.
4. preparation method according to claim 3, which is characterized in that the temperature for heating reaction is 600-1500 DEG C, heating
Time is 2-24 hours.
5. a kind of stratiform sulfoselenide as described in claim 1 as high rate capability sodium-ion battery positive material just
Application in the material composite of pole, which is characterized in that the positive electrode compound includes sodium-ion battery positive material, is also contained
There are conductive agent and binder, specifically: conductive agent and binder are added into sodium-ion battery positive material, then add solvent
(NMP) slurrying, smear are dry in blocks in conductive substrates, or add conductive agent into sodium-ion battery positive material and glue
Agent is tied, smear is directly dry-mixed tabletted in conductive substrates.
6. application according to claim 5, which is characterized in that the conductive agent be SPUER Li, S-O, KS-6, KS-15,
In SFG-6, SFG-15,350G, acetylene black (AB), Ketjen black (KB), gas-phase growth of carbon fibre (VGCF) or carbon nanotube (CNT)
One kind or in which several.
7. application according to claim 5, which is characterized in that the binder is polyvinyl alcohol (PVA), gathers inclined difluoro second
One of alkene (PVDF), polytetrafluoroethylene (PTFE) or sodium cellulose glycolate (CMC) are several.
8. application according to claim 5, which is characterized in that the drying condition be vacuum under or atmospheric conditions, do
50-150 DEG C of dry temperature, drying time 2-24 hour.
9. a kind of stratiform sulfoselenide as described in claim 1 as high rate capability sodium-ion battery positive material in sodium
Application in ion battery, which is characterized in that the sodium-ion battery, including as cathode metallic sodium or hard carbon material it is multiple
Close object, diaphragm, organic electrolyte and the sodium-ion battery positive material as anode.
10. a kind of sodium-ion battery positive material as described in claim 1 is preparing the application in energy energy storage device.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111193028A (en) * | 2020-01-08 | 2020-05-22 | 九江学院 | Preparation method of Fe-CrSe/C composite electrode material with nano structure |
| CN111916734A (en) * | 2020-07-09 | 2020-11-10 | 复阳固态储能科技(溧阳)有限公司 | Chromium-based sulfoselenide positive electrode material and preparation method and application thereof |
| CN113629245A (en) * | 2021-08-05 | 2021-11-09 | 肇庆市华师大光电产业研究院 | Novel compounding method of carbon material and transition metal compound, composite material and application |
| CN114039046A (en) * | 2021-11-02 | 2022-02-11 | 远景动力技术(江苏)有限公司 | Sodium ion battery and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111916734A (en) * | 2020-07-09 | 2020-11-10 | 复阳固态储能科技(溧阳)有限公司 | Chromium-based sulfoselenide positive electrode material and preparation method and application thereof |
| CN111916734B (en) * | 2020-07-09 | 2022-04-12 | 复阳固态储能科技(溧阳)有限公司 | Chromium-based sulfoselenide positive electrode material and preparation method and application thereof |
| CN113629245A (en) * | 2021-08-05 | 2021-11-09 | 肇庆市华师大光电产业研究院 | Novel compounding method of carbon material and transition metal compound, composite material and application |
| CN113629245B (en) * | 2021-08-05 | 2023-02-10 | 肇庆市华师大光电产业研究院 | Novel compounding method of carbon material and transition metal compound, composite material and application |
| CN114039046A (en) * | 2021-11-02 | 2022-02-11 | 远景动力技术(江苏)有限公司 | Sodium ion battery and preparation method thereof |
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