CN108110241A - A kind of classification carbon modification NaTi2(PO4)3The Preparation method and use of negative material - Google Patents
A kind of classification carbon modification NaTi2(PO4)3The Preparation method and use of negative material Download PDFInfo
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- CN108110241A CN108110241A CN201711366588.2A CN201711366588A CN108110241A CN 108110241 A CN108110241 A CN 108110241A CN 201711366588 A CN201711366588 A CN 201711366588A CN 108110241 A CN108110241 A CN 108110241A
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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
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—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
- H01M4/58—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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M2220/00—Batteries for particular applications
- H01M2220/10—Batteries in stationary systems, e.g. emergency power source in plant
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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
- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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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 provides a kind of classification carbon modification NaTi2(PO4)3The Preparation method and use of negative material, the preparation method include following preparation process, 1) sodium source, titanium source, phosphorus source are mixed, and add in carbon source, solvent and dispersant carry out high speed dispersion, obtain material A；2) material A is subjected to ball milling, obtains slurry B；3) material B is obtained into material C by spray drying；4) material C is heated up under an inert atmosphere, and the organic gas of cleavable at high temperature as carbon is passed through using certain flowing velocity, the NaTi of classification carbon modification is obtained after constant temperature calcining2(PO4)3Microballoon.The present invention efficiently solves NaTi2(PO4)3The problem of material electric conductivity is low considerably improves the electric conductivity of material, reduces internal resistance；Simple for process easy to control, feasibility is strong, volume production easy to implement.
Description
Technical field
The invention belongs to electrode material synthesis technical field, more particularly, to a kind of classification carbon modification NaTi2(PO4)3Cathode
The Preparation method and use of material.
Background technology
Greenization and the development of the sustainability energy have greatly promoted the innovation in terms of the energy, and there is an urgent need to one by people
Energy storage system of the kind with high-energy density is come the problem of alleviating using energy source aspect.Wherein, lithium ion battery is as one
The emerging energy storage system of kind is widely used in each electronic product, and has the gesture of fast development.In addition national policy side
The promotion of important breakthrough and industry in terms of the adjustment in face, scientific research has the lithium ion of higher energy density and long cycle characteristics
Battery will be more applied to the fields such as electric vehicle, extensive energy storage device, but lithium resource is in nature
Reserves are very limited, and lithium salts is expensive, limit application of the lithium ion battery in extensive energy storage.
In recent years, sodium-ion battery was since the advantages such as its abundant raw material, cheap were as global energy research field
Hot spot, and have good application prospect, electrode material conduct in large-scale energy storage device such as intelligent grid and electric vehicle
The key technology of sodium-ion battery development receives significant attention.Polyanionic compound titanium phosphate sodium NaTi2(PO4)3Material by
In its stabilization three-D space structure and with good ion transmission channel and chemical stability, charging/discharging voltage platform compared with
It is low, it is a kind of preferable negative material, but NaTi2(PO4)3The relatively low native electronic electrical conductivity of material causes the multiplying power of material
Poor-performing, capacity attenuation are very fast, seriously affect its commercialization process.
Therefore, it is necessary to provide a kind of NaTi2(PO4)3The preparation method of material, to improve the deficiency of current material.
The content of the invention
In view of this, the present invention is directed to propose a kind of classification carbon modification NaTi2(PO4)3The preparation method and use of negative material
On the way, to improve electrical conductivity, good chemical property is ensured.
In order to achieve the above objectives, the technical proposal of the invention is realized in this way：
A kind of classification carbon modification NaTi2(PO4)3The preparation method of negative material, including following preparation process,
1) sodium source, titanium source, phosphorus source are mixed, and adds in carbon source, solvent and dispersant and carry out high speed dispersion, obtained
Material A；
2) material A is subjected to ball milling, obtains slurry B；
3) material B is obtained into material C by spray drying；
4) material C is heated up under an inert atmosphere, and using certain flowing velocity be passed through at high temperature cleavable as
The organic gas of carbon obtains the NaTi of classification carbon modification after constant temperature calcining2(PO4)3Microballoon.
Preferably, in step 1), sodium source, titanium source, phosphorus source are according to molar ratio 0.95~1.05：1.9~2.1：2.85~
3.15 it is mixed；The addition of carbon source is the 5%~20% of material gross mass.
Preferably, in step 1), the sodium source includes：Sodium carbonate, sodium acid carbonate, sodium hydroxide, sodium sulphate, biphosphate
One or more in sodium, sodium chloride；
The titanium source includes：One or more in titanium tetrachloride, titanium dioxide, isopropyl titanate, butyl titanate；
Phosphorus source includes：Phosphoric acid, hypophosphorous acid, ammonium dihydrogen phosphate, sodium dihydrogen phosphate, potassium dihydrogen phosphate, phosphoric acid hydroxy ester
In one or more；
The carbon source includes：Glucose, citric acid, maltose, cellulose, polyethylene glycol, electrically conductive graphite, carbon nanotubes,
One or more in carbon black Super-p, graphite KS-6, graphene.
Preferably, in step 1), the solvent includes：One in water, ethyl alcohol, methanol, isopropanol, acetone, espeleton
Kind is a variety of；
The dispersant includes：In AA4040, oleyl amine, Sodium Polyacrylate, sodium pyrophosphate, dispersing agent MF
One or more.
Preferably, in step 2), Ball-milling Time is 2~6h.
Preferably, in step 3), the spray drying intake air temperature is 220~340 DEG C, air outlet temperature for 70~
120℃。
Preferably, in step 4), the inert gas includes：One kind or more in helium, nitrogen, argon gas, carbon dioxide
Kind；
The cleavable includes for the organic gas of carbon：In acetylene, methane, ethylene, ethane, propane, propylene, cyclopropane
One or more；
Preferably, material C is heated up under an inert atmosphere with the rate of heat addition of 1~10 DEG C/min in step 4), and
The organic gas of cleavable at high temperature as carbon is passed through using the flowing velocity of 0.5~10L/min, in 650~800 DEG C of constant temperature calcinings
8~12h.
The present invention also provides classification carbon prepared by method as described above to modify NaTi2(PO4)3Negative material, for carbon
The NaTi of embedded outer cladding structure2(PO4)3/ C complex microspheres, carbon content NaTi2(PO4)3/ C complex microsphere gross masses
10%~20%.
Present invention simultaneously provides a kind of cathode, the raw material components of the cathode include classification prepared by method as described above
Carbon modifies NaTi2(PO4)3Negative material.
Present invention simultaneously provides a kind of sodium-ion battery, the lithium ion battery includes point prepared by method as described above
Grade carbon modification NaTi2(PO4)3Negative material.
Compared with the prior art, a kind of classification carbon modification NaTi of the present invention2(PO4)3The preparation method of negative material
And purposes, it has the advantage that：
Sodium source, titanium source, phosphorus source and inorganic carbon source are uniformly mixed, are spray-dried using ball milling dispersing technology by the present invention
After obtain presoma, by a step intermediate sintering temperature method be successfully prepared high-carbon quantity classification modification NaTi2(PO4)3Microballoon.Ball milling
The scattered micron order mixing realized between raw material, NaTi is uniformly embedded by being sintered carbon2(PO4)3In sphere, simultaneously
The organic gas that cleavable is carbon is passed through in sintering process, forms cotton-shaped carbon coating in NaTi2(PO4)3It is prepared by spherome surface
Go out to embed the NaTi of outer cladding structure with carbon2(PO4)3/ C complex microspheres, carbon content is 10%~20%, and passes through carbon
Iris action can control microballoon primary particle size；High-carbon quantity classification modification shortens the transmission path of electrons/ions, effectively
Solves NaTi2(PO4)3The problem of material electric conductivity is low considerably improves the electric conductivity of material, reduces internal resistance；Medium temperature is burnt
Knot can avoid the side reaction that the carbon that high temperature occurs occurs with phosphate radical, and the soluble matter of reaction generation can seriously affect water system battery
Performance plays, and reduces sintering cost.Present invention process is simple and easy to control, and feasibility is strong, volume production easy to implement.
Specific embodiment
In addition to being defined, technical term used has universal with those skilled in the art of the invention in following embodiment
The identical meanings of understanding.Test reagent used, is routine biochemistry reagent unless otherwise specified in following embodiment；It is described
Experimental method is conventional method unless otherwise specified.
With reference to embodiment, the present invention will be described in detail.
Embodiment 1：
By sodium dihydrogen phosphate, titanium dioxide, ammonium dihydrogen phosphate according to molar ratio 1.04：2：3.15 are mixed, and according to
The 15% of material gross mass adds in 1.2% dispersant A A4040 of glucose and solid content, after according to material total amount 40%
Water is added to carry out high speed dispersion and obtains material A；Material A is subjected to ball milling, slurry is taken out after 3h, obtains material B, by material B with closing
Formula spraying is dried, and intake air temperature sets 260 DEG C, and air outlet temperature sets 90 DEG C, obtains material C；By material C in N2's
It is heated up under atmosphere with 2.5 DEG C/min, and acetylene gas is passed through with the flowing velocity of 1L/min, kept the temperature 8h at 800 DEG C, be classified
The NaTi of carbon modification2(PO4)3Microballoon.
The final carbon amounts of sample is 10.81% after tested, and powder electrical conductivity is 173.8 × 10-3S/cm。
Embodiment 2：
By sodium carbonate, titanium dioxide, potassium dihydrogen phosphate according to molar ratio 1.03：1.95：3.07 are mixed, and according to object
6% and the 10% of material gross mass is separately added into Super-p and polyethylene glycol and 1.8% dispersant A A4040 of solid content,
High speed dispersion is carried out according to material total amount 50% plus ethyl alcohol obtain material A afterwards；Material A is subjected to ball milling, slurry is taken out after 3h, obtains
To material B, the spraying of material B encloseds is dried, intake air temperature sets 260 DEG C, and air outlet temperature sets 100 DEG C, obtains
To material C；By material C in N2Atmosphere under heated up with 1.5 DEG C/min, and acetylene gas is passed through with the flowing velocity of 1L/min,
And 10h is kept the temperature at 780 DEG C, obtain the NaTi of classification carbon modification2(PO4)3Microballoon.
The final carbon amounts of sample is 13.53% after tested, and powder electrical conductivity is 391.3 × 10-3S/cm。
Embodiment 3：
By sodium hydroxide, titanium tetrachloride, potassium dihydrogen phosphate according to molar ratio 0.95：1.95：3 are mixed, and according to object
Material gross mass 6% and 4% is separately added into Super-p and KS-6 and 2% dispersant oleyl amine of solid content, after according to object
Material total amount 50% plus acetone carry out high speed dispersion and obtain material A；Material A is subjected to ball milling, slurry is taken out after 3.5h, obtains material
The spraying of material B encloseds is dried B, and intake air temperature sets 270 DEG C, and air outlet temperature sets 100 DEG C, obtains material
C；Material C under the atmosphere of Ar with 1.5 DEG C/min is heated up, and acetylene gas is passed through with the flowing velocity of 0.5L/min, and
780 DEG C of heat preservation 11h, obtain the NaTi of classification carbon modification2(PO4)3Microballoon.
The final carbon amounts of sample is 14.16% after tested, and powder electrical conductivity is 423.7 × 10-3S/cm。
Comparative example 1：
Sodium hydroxide, titanium dioxide, ammonium phosphate are shone into molar ratio 1：2：3 are mixed, and add in presoma and according to object
Expect that the 10% of gross mass adds in sucrose, after according to 30% plus water of material total amount carry out ball milling, take out slurry after 5h, sprayed with enclosed
Mist is dried, and intake air temperature sets 260 DEG C, and air outlet temperature sets 100 DEG C, material A is obtained, by material A in N2Gas
The lower 450 DEG C of constant temperature calcining 4h of atmosphere obtain material B, then again by material B in N2The lower 780 DEG C of constant temperature calcining 10h of atmosphere, obtain most
Final product, the final carbon amounts of sample is 5.17% after tested, and powder electrical conductivity is 7.17 × 10-3S/cm。
Performance test
The preparation of battery：
Respectively by titanium phosphate sodium material made from embodiment 1-3 and comparative example 1 according to active material：Conductive agent：Binding agent
=8:1:1 ratio uniform mixing, is coated on collector Thin Stainless Steel on piece, after drying, the cathode of battery is made；By LiMn2O4
Material is according to active material：Conductive agent 1：Conductive agent 2：Binding agent=75:10:5:10 ratio uniform mixing, is coated on afflux
In body titanium net, after drying, the anode of battery is made.Using non-woven fabrics as membrane, the Na of 1mol/L2SO4Solution is as electrolyte, group
Battery is dressed up, charge-discharge performance test is carried out to battery, charge and discharge are carried out with 2C current densities in the range of 0-1.8V.
1 sample chemical property of table
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modifications, equivalent replacements and improvements are made should all be included in the protection scope of the present invention god.
Claims (10)
1. a kind of classification carbon modification NaTi2(PO4)3The preparation method of negative material, which is characterized in that including following preparation process,
1) sodium source, titanium source, phosphorus source are mixed, and adds in carbon source, solvent and dispersant and carry out high speed dispersion, obtain material
A；
2) material A is subjected to ball milling, obtains slurry B；
3) material B is obtained into material C by spray drying；
4) material C is heated up under an inert atmosphere, and using certain flowing velocity be passed through at high temperature cleavable as carbon
Organic gas obtains the NaTi of classification carbon modification after constant temperature calcining2(PO4)3Microballoon.
2. classification carbon modification NaTi according to claim 12(PO4)3The preparation method of negative material, it is characterised in that：Step
It is rapid 1) in, sodium source, titanium source, phosphorus source are according to molar ratio 0.95~1.05：1.9~2.1：2.85~3.15 are mixed；Carbon source
Addition is the 5%~20% of material gross mass.
3. classification carbon modification NaTi according to claim 1 or 22(PO4)3The preparation method of negative material, feature exist
In：In step 1), the sodium source includes：In sodium carbonate, sodium acid carbonate, sodium hydroxide, sodium sulphate, sodium dihydrogen phosphate, sodium chloride
One or more；
The titanium source includes：One or more in titanium tetrachloride, titanium dioxide, isopropyl titanate, butyl titanate；
Phosphorus source includes：In phosphoric acid, hypophosphorous acid, ammonium dihydrogen phosphate, sodium dihydrogen phosphate, potassium dihydrogen phosphate, phosphoric acid hydroxy ester
It is one or more；
The carbon source includes：Glucose, citric acid, maltose, cellulose, polyethylene glycol, electrically conductive graphite, carbon nanotubes, carbon black
One or more in Super-p, graphite KS-6, graphene.
4. classification carbon modification NaTi according to claim 1 or 22(PO4)3The preparation method of negative material, feature exist
In：In step 1), the solvent includes：One or more in water, ethyl alcohol, methanol, isopropanol, acetone, espeleton；
The dispersant includes：One in AA4040, oleyl amine, Sodium Polyacrylate, sodium pyrophosphate, dispersing agent MF
Kind is a variety of.
5. classification carbon modification NaTi according to claim 1 or 22(PO4)3The preparation method of negative material, feature exist
In：In step 2), Ball-milling Time is 2~6h.
6. the classification carbon modification NaTi described in claim 1 or 22(PO4)3The preparation method of negative material, it is characterised in that：Step
It is rapid 3) in, it is described spray drying intake air temperature be 220~340 DEG C, air outlet temperature be 70~120 DEG C.
7. the classification carbon modification NaTi described in claim 1 or 22(PO4)3The preparation method of negative material, it is characterised in that：Step
It is rapid 4) in, the inert gas includes：One or more in helium, nitrogen, argon gas, carbon dioxide；
The cleavable includes for the organic gas of carbon：One in acetylene, methane, ethylene, ethane, propane, propylene, cyclopropane
Kind is a variety of；
Preferably, material C is heated up under an inert atmosphere with the rate of heat addition of 1~10 DEG C/min in step 4), and with 0.5
The flowing velocity of~10L/min is passed through the organic gas that cleavable at high temperature is carbon, in 650~800 DEG C of constant temperature calcinings 8~
12h。
8. the classification carbon prepared according to claim 1~7 any one of them method modifies NaTi2(PO4)3Negative material, it is special
Sign is, to embed the NaTi of outer cladding structure with carbon2(PO4)3/ C complex microspheres, carbon content NaTi2(PO4)3/ C is multiple
Close the 10%~20% of microballoon gross mass.
9. a kind of cathode, which is characterized in that the raw material components of the cathode include such as claim 1~7 any one of them side
Classification carbon modification NaTi prepared by method2(PO4)3Negative material.
10. a kind of sodium-ion battery, which is characterized in that the lithium ion battery includes such as claim 1~7 any one of them
Classification carbon modification NaTi prepared by method2(PO4)3Negative material.
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| CN109599547A (en) * | 2018-12-07 | 2019-04-09 | 贝特瑞（天津）纳米材料制造有限公司 | NaTi2(PO4)3-TiO2Preparation method and application of/C composite electrode material |
| CN110783621A (en) * | 2019-10-18 | 2020-02-11 | 扬州扬达新能源有限公司 | Water system sodium ion battery and preparation method thereof |
| WO2020210371A1 (en) * | 2019-04-08 | 2020-10-15 | Benan Energy | Methods for ntp manufacturing |
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