CN108539125A - A kind of high-energy density lithium sulphur power battery preparation method and battery - Google Patents
A kind of high-energy density lithium sulphur power battery preparation method and battery Download PDFInfo
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- CN108539125A CN108539125A CN201810359416.0A CN201810359416A CN108539125A CN 108539125 A CN108539125 A CN 108539125A CN 201810359416 A CN201810359416 A CN 201810359416A CN 108539125 A CN108539125 A CN 108539125A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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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- 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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- Chemical Kinetics & Catalysis (AREA)
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- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
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Abstract
The invention discloses a kind of high-energy density lithium sulphur power battery preparation method and batteries, by metallic lithium layer compacting in foam copper, the pore structure of foam copper can alleviate the formation of lithium-sulfur cell Li dendrite, it avoids Li dendrite and pierces through diaphragm, improve the security performance of battery, the diaphragm bag of this external application one end open encapsulates foam copper/cathode of lithium pole piece, obtain hermetically sealed junior unit, it on the one hand can be to avoid short circuit problem caused by the positive and negative anodes dislocation occurred by diaphragm fold during lamination, it on the other hand being in direct contact to avoid metallic lithium layer during lamination and air or oxygen.
Description
Technical field
The invention belongs to field of lithium, specifically, being related to a kind of high-energy density lithium sulphur power battery preparation method
And battery.
Background technology
As environmental problem is increasingly severe and policy guidance, global every country policies several years successively
After will forbid selling fuel vehicle instead New-energy electric vehicle.Therefore new-energy automobile is the current automobile neck in China
The only way which must be passed of domain development, needs to strengthen research and development capabilities, and develops the new product for being suitble to current demand.Over the past two years, the new energy of China
Source market rapid growth, each vehicle enterprise also begin to carry out new-energy automobile energetically.
Power battery is the core of electric vehicle and the key component that can new-energy automobile fast-developing.Root
It is required according to national policy, the year two thousand twenty power battery monomer reaches 350Wh/kg than energy, and power battery monomer is reached than energy within 2025
400Wh/kg, the year two thousand thirty power battery monomer reach 500Wh/kg than energy.It is moved at this stage with the lithium ion that ternary material is anode
Power battery, energy density only have 200Wh/kg~280Wh/kg, and course continuation mileage is less than 350 kilometers, in current nickelic NCM, NCA
In the case of positive electrode cyclical stability difference, it is difficult to realize above-mentioned target in a short time.Therefore lithium-ion-power cell energy is improved
Density reduces cost simultaneously, is current new-energy automobile to promote new-energy automobile course continuation mileage and power battery service life
Develop technical problem urgently to be resolved hurrily.
In view of this special to propose the present invention.
Invention content
It is dynamic that the technical problem to be solved in the present invention is to overcome the deficiencies of the prior art and provide a kind of high-energy density lithium sulphur
Power battery preparation method and battery.
In order to solve the above technical problems, the present invention is using the basic conception of technical solution：
A kind of high-energy density lithium sulphur power battery preparation method, preparation process include the preparation, just of positive active material
The preparation of pole slurry, the preparation of negative plate/diaphragm, the preparation of positive plate, battery assembly, which is characterized in that the positive-active
Substance is prepared as：High-temperature calcination twice is carried out by tube furnace using after sepiolite and elemental sulfur mixing, is crushed.
Further, the negative plate/diaphragm is prepared as：Foam copper is embedded in metallic lithium layer, under inert atmosphere, high pressure
It is compacted, and is encapsulated using the diaphragm bag of one end open.
Further, in the preparation process of the positive plate, aluminium foil surface coats the carbon nanotube of one layer of array.
Further, in the preparation process of the positive active material, the mass ratio of sepiolite and elemental sulfur is：2~3:7
~8, the fineness of the elemental sulfur is less than 1 μm, and purity is more than 99.9%.
Further, in the preparation process of the positive active material, in tube furnace atmospheric condition be vacuum or N2 atmosphere,
The condition of high-temperature calcination twice is respectively：150~200 DEG C, 300-350 DEG C, the grain size of the positive active material is less than 15 μm.
Further, in the preparation process of the negative plate/diaphragm, foam copper thickness is 15~20 μm, pressure 15Kg/
cm2。
Further, in the preparation process of the negative plate/diaphragm, diaphragm bag forms three edge sealings on one side by two layers of diaphragm
The sack of opening, single-layer septum thickness are 20~25 μm.
Further, in the preparation process of the positive plate, carbon nanotube thickness is 12~16 μm.
A kind of high-energy density lithium sulphur power battery is prepared with above-mentioned high-energy density lithium sulphur power battery preparation method
It forms.
After adopting the above technical scheme, the present invention has the advantages that compared with prior art.
1, by metallic lithium layer compacting in foam copper, the pore structure of foam copper can alleviate the shape of lithium-sulfur cell Li dendrite
At, avoid Li dendrite pierce through diaphragm, improve the security performance of battery.
2, foam copper/cathode of lithium pole piece is encapsulated with the diaphragm bag of one end open, obtains hermetically sealed junior unit, on the one hand may be used
It, on the other hand can be to avoid folded to avoid short circuit problem caused by the positive and negative anodes dislocation occurred by diaphragm fold during lamination
Metallic lithium layer and air or oxygen is in direct contact during piece.
3, the carbon nanotube that one layer of array is coated in aluminium foil surface, can solve the problems, such as elemental sulfur poorly conductive, into one
Step improves the load sulfur content of anode, to improve the energy density of system.
4, sepiolite is a kind of rich magnesium silicate clay mineral, resourceful, cheap, can reduce battery at
This.
5, under the premise of ensureing to use safely, the energy density of lithium sulphur electrical core of power battery can be increased to 500Wh/kg with
On, at 25 DEG C of room temperature, 1C charge and discharge cycles are carried out, 500 cycle capacity retention ratio of charge and discharge cycles is up to 85% or more.
The specific implementation mode of the present invention is described in further detail below in conjunction with the accompanying drawings.
Description of the drawings
A part of the attached drawing as the application, for providing further understanding of the invention, of the invention is schematic
Embodiment and its explanation do not constitute inappropriate limitation of the present invention for explaining the present invention.Obviously, the accompanying drawings in the following description
Only some embodiments to those skilled in the art without creative efforts, can be with
Other accompanying drawings can also be obtained according to these attached drawings.In the accompanying drawings：
Fig. 1 is battery charging and discharging curve graph in the embodiment of the present invention one；
Fig. 2 is a kind of circulating battery curve graph of the embodiment of the present invention.
It should be noted that these attached drawings and verbal description are not intended to the design model limiting the invention in any way
It encloses, but is that those skilled in the art illustrate idea of the invention by referring to specific embodiments.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, the technical solution in embodiment is clearly and completely described, following embodiment for illustrating the present invention, but
It is not limited to the scope of the present invention.
In the description of the present invention, it should be noted that term "upper", "front", "rear", "left", "right", " is erected at "lower"
Directly ", the orientation or positional relationship of the instructions such as "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, merely to just
In the description present invention and simplify description, do not indicate or imply the indicated device or element must have a particular orientation, with
Specific azimuth configuration and operation, therefore be not considered as limiting the invention.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
Can also be electrical connection to be mechanical connection；It can be directly connected, it can also be indirectly connected through an intermediary.For this
For the those of ordinary skill in field, the concrete meaning of above-mentioned term in the present invention can be understood with concrete condition.
Embodiment one
Step S1：The preparation of sulfur-bearing positive active material
According to weight percent 75%：25% weighs elemental sulfur, sepiolite respectively, and first carrying out preliminary mixing keeps elemental sulfur equal
It is even to be blended in sepiolite, then mixed grinding 3h in the ball mill, then mixed powder is put into tube furnace, in vacuum or
Temperature is set as 155 DEG C under N2 atmosphere, calcines 3h；320 DEG C are further warming up to, 1h is calcined, to remove blending surface not
Incorporate the elemental sulfur entered；It finally crushes to obtain sepiolite/sulphur composite material of the grain size less than 15 μm using pulverizer.
Step S2：The preparation of anode sizing agent
First according to weight percent 89%：7.5%：3.5% weigh respectively sepiolite/sulphur composite material, acetylene black,
PVDF, then solvent NMP is weighed in the ratio of glue solid content 6%, 40 revs/min of mixing speed, 35 revs/min of rate of dispersion, 3h is obtained
To the glue of homogeneous transparent；Then conductive agent acetylene black is added according to 35 revs/min of mixing speed, 35 revs/min of rate of dispersion, operation
1h；；It is eventually adding sepiolite/sulphur composite material, according to 35 revs/min of mixing speed, 30 revs/min of rate of dispersion, operation 4h is obtained
Anode sizing agent, anode sizing agent solid content are 67.7%, and viscosity 9200mpa.s, slurry fineness is about 25 μm.
Step S3：The preparation of negative plate/diaphragm
Embedded metallic lithium layer 7 passes through high pressure 15Kg/cm under an inert atmosphere among two layers of porous foam copper 82
Compacting obtains foam copper/lithium cathode sheet 12, then 12 plug flat of foam copper/lithium cathode sheet is entered to the diaphragm bag 4 of one end open, finally will
Cathode/diaphragm junior unit 13 is made in open end hot pressing closure.
Step S4：Positive plate makes
The step S2 anode sizing agents prepared are coated uniformly in utter misery aluminum foil current collector, aluminium foil surface coats a thickness 12
The carbon nanotube of~16 μm of arrays, through overbaking, roll-in is die cut and required anode pole piece is made.
Step S5：Battery assembles
Cathode obtained by step S3 and step S4/diaphragm junior unit and anode pole piece are stacked into naked battery core, then will be naked
Battery core is put into aluminum plastic film sealing shell, is eventually adding LiNO containing additive3The electrolyte that proportion is 6.0% seal to obtain 25Ah at
Product battery core.
Comparative example：
Step S1：The preparation of sulfur-bearing positive active material
According to weight percent 75%：25% weighs elemental sulfur, sepiolite respectively, and first carrying out preliminary mixing keeps elemental sulfur equal
It is even to be blended in sepiolite, then mixed grinding 3h in the ball mill, then mixed powder is put into tube furnace, in vacuum or
Temperature is set as 155 DEG C under N2 atmosphere, calcines 3h；320 DEG C are further warming up to, 1h is calcined, to remove blending surface not
Incorporate the elemental sulfur entered；It finally crushes to obtain sepiolite/sulphur composite material of the grain size less than 15 μm using pulverizer.
Step S2：The preparation of anode sizing agent
First according to weight percent 89%：7.5%：3.5% weigh respectively sepiolite/sulphur composite material, acetylene black,
PVDF, then solvent NMP is weighed in the ratio of glue solid content 6%, 40 revs/min of mixing speed, 35 revs/min of rate of dispersion, 3h is obtained
To the glue of homogeneous transparent；Then conductive agent acetylene black is added according to 35 revs/min of mixing speed, 35 revs/min of rate of dispersion, operation
1h；；It is eventually adding sepiolite/sulphur composite material, according to 35 revs/min of mixing speed, 30 revs/min of rate of dispersion, operation 4h is obtained
Anode sizing agent, anode sizing agent solid content are 67.7%, and viscosity 9200mpa.s, slurry fineness is about 25 μm.
Step S3：The preparation of negative plate/diaphragm
One layer of lithium layer is coated on copper foil of affluxion body surface, required cathode pole piece is made.
Step S4：Positive plate makes
The step S2 anode sizing agents prepared are coated uniformly in utter misery aluminum foil current collector, through overbaking, roll-in, cross cutting system
Obtain required anode pole piece.
Step 5：Battery assembles
The side using lamination will be separated among cathode pole piece and anode pole piece obtained by step S3 and step S4 with diaphragm
Formula prepares naked battery core, then naked battery core is put into aluminum plastic film sealing shell, and it is 6.0% to be eventually adding the proportions of LiNO3 containing additive
Electrolyte seals to obtain 25Ah finished product battery cores.
Electrochemical reaction just has occurred in the lithium sulphur power battery of the present invention after fluid injection, i.e. cathode Li+ enters electrolyte, so
It by foam copper, diaphragm or is directly over diaphragm bag afterwards and reaches side of the positive electrode, therefore the lithium-sulfur cell needs first to discharge and charge afterwards.Therefore
Provide that the lithium sulphur power battery formation process is that first constant-current discharge is electric to charge cutoff to discharge cut-off voltage, then constant-current charge
Pressure.
The lithium sulphur power battery formation process flow of the present invention is as follows
1,3min is stood；
2,0.005C constant-current discharges 150min, blanking voltage 1.7V
3,3min is stood；
4,0.01C constant-current discharges 150min, blanking voltage 1.7V
5,3min is stood；
6,0.05C constant-current discharges 120min, blanking voltage 1.7V
7,3min is stood；
8,0.2C constant-current discharges 120min, blanking voltage 1.7V
9,3min is stood；
10,0.5C constant-current discharges are to blanking voltage 1.7V
11,30min is stood；
12,0.005C constant-current charges, blanking voltage 2.0V
13,10min is stood；
14,0.01C constant-current charges, blanking voltage 2.3V
15,10min is stood；
16,0.05C constant-current charges, blanking voltage 2.5V
17,10min is stood；
18,0.18C constant-current charges, blanking voltage 2.8V
Experimental contrast analysis
It is each to the finished product battery core obtained by embodiment 1 and comparative example in order to further illustrate the technique effect of the present embodiment
Sampling 1000 tests its security performance by short-circuit test, and record data are as shown in following table one.
By one data of table as it can be seen that the disqualification rate caused by short circuit can be reduced using this embodiment scheme 1, significantly improve
The security performance and qualification rate of product
Charge-discharge test is carried out according to 1 gained lithium sulphur power battery of embodiment, lithium sulphur power battery of the present invention is filled at 1C
Discharge curve such as Fig. 1, the nominal voltage for thus providing lithium sulphur power battery of the present invention are 2.0V.
According to lithium sulphur power battery obtained by embodiment, at 25 DEG C of room temperature, 1C charge and discharge cycles are carried out, charge and discharge cycles are bent
Line under 1C multiplying powers as shown in Fig. 2, recycle 500 weeks capacity retention ratios up to 85% or more.
The above is only presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this patent
Member without departing from the scope of the present invention, when the technology contents using above-mentioned prompt make it is a little change or be modified to
The equivalent embodiment of equivalent variations, it is right according to the technical essence of the invention as long as being the content without departing from technical solution of the present invention
Any simple modification, equivalent change and modification made by above example, in the range of still falling within the present invention program.
Claims (10)
1. a kind of high-energy density lithium sulphur power battery preparation method, preparation process include the preparation of positive active material, anode
The preparation of slurry, the preparation of negative plate/diaphragm, the preparation of positive plate, battery assembly, which is characterized in that the positive electrode active material
Matter is prepared as：High-temperature calcination twice is carried out by tube furnace using after sepiolite and elemental sulfur mixing, is crushed.
2. high-energy density lithium sulphur power battery preparation method according to claim 1, which is characterized in that the cathode
Piece/diaphragm is prepared as：Foam copper is embedded in metallic lithium layer, under inert atmosphere, high pressure compression forms, and using one end open
Diaphragm bag encapsulates.
3. high-energy density lithium sulphur power battery preparation method according to claim 1, which is characterized in that the positive plate
Preparation process in, aluminium foil surface coat one layer of array carbon nanotube.
4. high-energy density lithium sulphur power battery preparation method according to claim 1, which is characterized in that the anode is living
In the preparation process of property substance, the mass ratio of sepiolite and elemental sulfur is：2~3:7~8.
5. high-energy density lithium sulphur power battery preparation method according to claim 4, which is characterized in that the elemental sulfur
Fineness be less than 1 μm, purity be more than 99.9%.
6. high-energy density lithium sulphur power battery preparation method according to claim 1, which is characterized in that the anode is living
Property substance preparation process in, atmospheric condition is vacuum or N2 atmosphere in tube furnace, and the condition of high-temperature calcination twice is respectively：
150~200 DEG C, 300-350 DEG C.
7. high-energy density lithium sulphur power battery preparation method according to claim 6, which is characterized in that the anode is living
Property substance grain size be less than 15 μm.
8. high-energy density lithium sulphur power battery preparation method according to claim 2, which is characterized in that the cathode
In the preparation process of piece/diaphragm, foam copper thickness is 15~20 μm, pressure 15Kg/cm2。
9. high-energy density lithium sulphur power battery preparation method according to claim 2, which is characterized in that the cathode
In the preparation process of piece/diaphragm, diaphragm bag is made of the sack of three edge sealing openings at one side two layers of diaphragm, and single-layer septum thickness is
20~25 μm.
10. high-energy density lithium sulphur power battery preparation method according to claim 3, which is characterized in that the anode
In the preparation process of piece, carbon nanotube thickness is 12~16 μm.
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