CN110336025A - A kind of lithium sulfur battery anode material and preparation method thereof - Google Patents
A kind of lithium sulfur battery anode material and preparation method thereof Download PDFInfo
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- CN110336025A CN110336025A CN201910577951.8A CN201910577951A CN110336025A CN 110336025 A CN110336025 A CN 110336025A CN 201910577951 A CN201910577951 A CN 201910577951A CN 110336025 A CN110336025 A CN 110336025A
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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
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/621—Binders
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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 invention discloses a kind of lithium sulfur battery anode materials, it includes each raw material of following weight parts: sulphur 75-85, electrically conductive graphite 1-5, conductive agent solution 250-300, adhesive 8-15, the present invention can alleviate the problem of sulphur volume expansion in charge and discharge process, and play the role of physical limit to the dissolution of polysulfide shuttle, so as to effectively improve specific capacity, high rate performance and the cyclical stability of lithium-sulfur cell.
Description
Technical field
The invention belongs to battery material fields, and in particular to a kind of lithium sulfur battery anode material and preparation method thereof.
Background technique
Lithium-sulfur cell be using sulphur as positive active material, using lithium as the secondary cell of cathode, wherein positive active material sulphur
Theoretical specific capacity it is higher, but the complicated electrochemical reaction process of sulfur-bearing anode and its physical properties such as non-conductive determine lithium
The research and development difficult point of sulphur battery is mainly in positive electrode.For the application for realizing lithium-sulfur cell, leading for positive electrode is on the one hand improved
Electric rate improves the high rate performance of battery to improve the utilization rate of positive active material；On the other hand also to inhibit capacity can not
Inverse loss, to improve the cycle performance of battery；
Lithium-sulfur cell is concerned in recent years because it has the advantages that high theoretical energy density, environmental pollution are small.But
Still there are some defects in the lithium-sulfur cell developed at present, e.g., lithium-sulfur cell can generate shuttle effect in charge and discharge process
It answers, causes the irreversible loss of active material, battery capacity is caused to decay；Lithium-sulfur cell generates in charge and discharge process simultaneously
More lithium sulfides, so that cathode of lithium has Li dendrite generation, the cyclical stability of lithium-sulfur cell can be caused to be deteriorated in cathode deposition.
Summary of the invention
The object of the present invention is to provide a kind of lithium sulfur battery anode materials and preparation method thereof.
To achieve the above object, the invention adopts the following technical scheme:
A kind of lithium sulfur battery anode material, it includes each raw material of following weight parts:
Sulphur 75-85, electrically conductive graphite 1-5, conductive agent solution 250-300, adhesive 8-15.
The raw material composition of the conduction agent solution following weight parts:
Diethylenetriamine 2-3, thiophene 15-20, ferric chloride (FeCl36H2O) 0.4-2, carbon nanotube 60-70, sodium acrylate 20-
30, ammonium persulfate 0.6-1, aluminium dihydrogen phosphate 2-4, polysorbate 0.4-1.
The preparation method of the conduction agent solution, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly；
(2) diethylenetriamine is taken, is added in the dehydrated alcohol of 10-14 times of mixture weight, stirs evenly, thiophene is added
Pheno, increasing temperature is 55-60 DEG C, insulated and stirred 1-2 hours, obtains amine aqueous solution；
(3) ferric chloride (FeCl36H2O) is taken, is added in the deionized water of 10-19 times of its weight, stirs evenly, it is molten to obtain oxidant
Liquid；
(4) carbon nanotube is taken, is added in the nitric acid solution that concentration is 96-98%, 10-13 hours ultrasonic, filtering will sink
It forming sediment and washes, air drying mixes with sodium acrylate, is added in the deionized water of 20-26 times of mixture weight, stirs evenly,
It is sent in reaction kettle, is passed through nitrogen, adjusting temperature of reaction kettle is 65-70 DEG C, and insulated and stirred 4-5 hours, it is molten that above-mentioned amine is added
Liquid, polysorbate, reducing temperature of reaction kettle is 10-15 DEG C, is added above-mentioned oxidizing agent solution, insulated and stirred 10-15 hours, out
Material, mixes with aluminium dihydrogen phosphate, stirs evenly to get the conductive agent solution.
The preparation method of described adhesive, comprising the following steps:
The phenol of 40-50 parts by weight, the propylene oxide mixing of 2-3 parts by weight are taken, 10-14 times of mixture weight is added to
It in dehydrated alcohol, stirs evenly, increasing temperature is 50-60 DEG C, and insulated and stirred 1-2 hours, the 37% of 70-75 parts by weight is added
Formaldehyde stirs evenly, and is sent in 85-90 DEG C of water bath with thermostatic control, and the sodium hydroxide of 10-15 parts by weight, insulated and stirred 3-4 is added
Hour, it discharges, filters, filter cake is washed, insulated and stirred 20-30 minutes at 60-65 DEG C, is cooled to room temperature to get the bonding
Agent.
The concentration of the sodium hydroxide is 0.7-1mol/l.
A kind of preparation method of lithium sulfur battery anode material, comprising the following steps:
Sulphur is taken, is added in conductive agent solution, increasing temperature is 40-50 DEG C, and 4-6 hours ultrasonic, filtering will precipitate water
It washes, is sent in sintering furnace after dry, adhesive is added, increasing temperature is 170-175 DEG C, keeps the temperature 40-50 minutes, is passed through argon gas
Protection, reducing temperature is 140-150 DEG C, and insulated and stirred 12-15 hours, discharging was cooled to room temperature to get the lithium-sulfur cell just
Pole material.
Advantages of the present invention:
Conductive agent of the invention is compound with polythiophene and carbon nanotube, and aluminium dihydrogen phosphate will gather first as hot adhesive
Sodium acrylate is distributed between carbon nanotube by way of monomer polymerization, and Sodium Polyacrylate has good adhesive property,
It, can be by obtained polythiophene particle absorption between carbon nanotube, and likewise, passing through introducing again in the polymerization of thiophene monomer
Adhesive containing epoxy group, is blended with sulphur, and aluminium dihydrogen phosphate plays a role as hot adhesive, cooperates with epoxy cross-linking,
Also promote dispersion of the sulphur between carbon nanotube, and pass through hot adhesion after dispersing, stationarity is strong, can alleviate sulphur in charge and discharge process
The problem of volume expansion, and play the role of physical limit to the dissolution of polysulfide shuttle, so as to effectively improve lithium
Specific capacity, high rate performance and the cyclical stability of sulphur battery.
Specific embodiment
Embodiment 1
A kind of lithium sulfur battery anode material, it includes each raw material of following weight parts:
Sulphur 85, electrically conductive graphite 5, conductive agent solution 250, adhesive 15.
The raw material composition of the conduction agent solution following weight parts:
Diethylenetriamine 3, thiophene 20, ferric chloride (FeCl36H2O) 2, carbon nanotube 70, sodium acrylate 30, ammonium persulfate 1, phosphoric acid
Aluminum dihydrogen 4, polysorbate 1.
The preparation method of the conduction agent solution, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 30 times of its weight, stirs evenly；
(2) diethylenetriamine is taken, is added in 14 times of mixture weight of dehydrated alcohol, stirs evenly, thiophene is added, is risen
High-temperature is 60 DEG C, insulated and stirred 2 hours, obtains amine aqueous solution；
(3) ferric chloride (FeCl36H2O) is taken, is added in the deionized water of 19 times of its weight, is stirred evenly, obtain oxidizing agent solution；
(4) carbon nanotube is taken, is added in the nitric acid solution that concentration is 96-98%, ultrasound 13 hours, filtering will precipitate
Washing, air drying mix with sodium acrylate, are added in 26 times of mixture weight of deionized water, stir evenly, be sent to
In reaction kettle, it is passed through nitrogen, adjusting temperature of reaction kettle is 70 DEG C, insulated and stirred 5 hours, above-mentioned amine aqueous solution, polysorbate is added,
Reducing temperature of reaction kettle is 15 DEG C, and above-mentioned oxidizing agent solution is added, and insulated and stirred 15 hours, discharging was mixed with aluminium dihydrogen phosphate,
It stirs evenly to get the conductive agent solution.
The preparation method of described adhesive, comprising the following steps:
The phenol of 50 parts by weight, the propylene oxide mixing of 2-3 parts by weight are taken, 14 times of mixture weight of anhydrous second is added to
In alcohol, stir evenly, increasing temperature is 50 DEG C, insulated and stirred 2 hours, 37% formaldehyde of 75 parts by weight is added, stirs evenly,
It is sent in 90 DEG C of water bath with thermostatic control, the sodium hydroxide of 15 parts by weight is added, insulated and stirred 4 hours, discharges, filters, by filter cake
It washes, insulated and stirred 30 minutes at 65 DEG C, is cooled to room temperature to get described adhesive.
The concentration of the sodium hydroxide is 1mol/l.
A kind of preparation method of lithium sulfur battery anode material, comprising the following steps:
Sulphur is taken, is added in conductive agent solution, increasing temperature is 50 DEG C, ultrasound 6 hours, and precipitating is washed in filtering, dry
After be sent in sintering furnace, be added adhesive, increase temperature be 175 DEG C, keep the temperature 50 minutes, be passed through argon gas protection, reduce temperature
It is 150 DEG C, insulated and stirred 15 hours, discharging was cooled to room temperature to get the lithium sulfur battery anode material.
Embodiment 2
A kind of lithium sulfur battery anode material, it includes each raw material of following weight parts:
Sulphur 75, electrically conductive graphite 1, conductive agent solution 300, adhesive 8.
The raw material composition of the conduction agent solution following weight parts:
Diethylenetriamine 2, thiophene 15, ferric chloride (FeCl36H2O) 0.4, carbon nanotube 60, sodium acrylate 20, ammonium persulfate 0.6,
Aluminium dihydrogen phosphate 2, polysorbate 0.4.
The preparation method of the conduction agent solution, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 20 times of its weight, stirs evenly；
(2) diethylenetriamine is taken, is added in 10 times of mixture weight of dehydrated alcohol, stirs evenly, thiophene is added, is risen
High-temperature is 55 DEG C, insulated and stirred 1 hour, obtains amine aqueous solution；
(3) ferric chloride (FeCl36H2O) is taken, is added in the deionized water of 10 times of its weight, is stirred evenly, obtain oxidizing agent solution；
(4) carbon nanotube is taken, is added in the nitric acid solution that concentration is 96%, ultrasound 10 hours, filtering will precipitate water
It washes, air drying is mixed with sodium acrylate, is added in 20 times of mixture weight of deionized water, is stirred evenly, and is sent to anti-
It answers in kettle, is passed through nitrogen, adjusting temperature of reaction kettle is 65 DEG C, and insulated and stirred 4 hours, above-mentioned amine aqueous solution, polysorbate is added, and is dropped
Low reaction kettle temperature degree is 10 DEG C, above-mentioned oxidizing agent solution is added, insulated and stirred 10-15 hours, discharging was mixed with aluminium dihydrogen phosphate
It closes, stirs evenly to get the conductive agent solution.
The preparation method of described adhesive, comprising the following steps:
The phenol of 40 parts by weight, the propylene oxide mixing of 2 parts by weight are taken, 10 times of mixture weight of dehydrated alcohol is added to
In, it stirs evenly, increasing temperature is 50 DEG C, insulated and stirred 1 hour, 37% formaldehyde of 70 parts by weight is added, stirs evenly, send
Enter into 85 DEG C of water bath with thermostatic control, the sodium hydroxide of 10 parts by weight is added, insulated and stirred 3-4 hours, discharges, filters, by filter cake
It washes, insulated and stirred 20 minutes at 60 DEG C, is cooled to room temperature to get described adhesive.
The concentration of the sodium hydroxide is 0.7mol/l.
A kind of preparation method of lithium sulfur battery anode material, comprising the following steps:
Sulphur is taken, is added in conductive agent solution, increasing temperature is 40 DEG C, ultrasound 4 hours, and precipitating is washed in filtering, dry
After be sent in sintering furnace, be added adhesive, increase temperature be 170 DEG C, keep the temperature 40 minutes, be passed through argon gas protection, reduce temperature
It is 140 DEG C, insulated and stirred 12 hours, discharging was cooled to room temperature to get the lithium sulfur battery anode material.
Performance test:
Lithium-sulfur cell is prepared using lithium sulfur battery anode material prepared by the embodiment of the present invention 1, embodiment 2, is then existed
2.08~2.35V voltage range carries out 300 circle constant current charge-discharge circulations, and 0.1C charging/0.1C electric discharge measures each sulphur lithium battery
The capacity of sulphur lithium battery, testing result after first discharge specific capacity, 500 circle of circulation specifically:
Lithium-sulfur cell prepared by the embodiment of the present invention 1:
First discharge specific capacity: the specific capacity 1177mAh/g of sulphur lithium battery after 1450mAh/g, 500 circle of circulation；Capacity is protected
Holdup: 81.17%；
Lithium-sulfur cell prepared by the embodiment of the present invention 2:
First discharge specific capacity: the specific capacity 1150mAh/g of sulphur lithium battery after 1390mAh/g, 500 circle of circulation；Capacity is protected
Holdup: 82.73%.
Claims (6)
1. a kind of lithium sulfur battery anode material, which is characterized in that it includes each raw material of following weight parts:
Sulphur 75-85, electrically conductive graphite 1-5, conductive agent solution 250-300, adhesive 8-15.
2. a kind of lithium sulfur battery anode material according to claim 1, which is characterized in that the conduction agent solution is following heavy
Measure the raw material composition of part:
Diethylenetriamine 2-3, thiophene 15-20, ferric chloride (FeCl36H2O) 0.4-2, carbon nanotube 60-70, sodium acrylate 20-30, mistake
Ammonium sulfate 0.6-1, aluminium dihydrogen phosphate 2-4, polysorbate 0.4-1.
3. a kind of lithium sulfur battery anode material according to claim 2, which is characterized in that the preparation of the conduction agent solution
Method, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly；
(2) diethylenetriamine is taken, is added in the dehydrated alcohol of 10-14 times of mixture weight, stirs evenly, thiophene is added, is risen
High-temperature is 55-60 DEG C, insulated and stirred 1-2 hours, obtains amine aqueous solution；
(3) ferric chloride (FeCl36H2O) is taken, is added in the deionized water of 10-19 times of its weight, stirs evenly, obtain oxidizing agent solution；
(4) carbon nanotube is taken, is added in the nitric acid solution that concentration is 96-98%, 10-13 hours ultrasonic, filtering will precipitate water
It washes, air drying is mixed with sodium acrylate, is added in the deionized water of 20-26 times of mixture weight, is stirred evenly, and is sent into
Into reaction kettle, it is passed through nitrogen, adjusting temperature of reaction kettle is 65-70 DEG C, insulated and stirred 4-5 hours, above-mentioned amine aqueous solution is added, gathers
Sorb ester, reducing temperature of reaction kettle is 10-15 DEG C, and above-mentioned oxidizing agent solution is added, insulated and stirred 10-15 hours, discharges, with phosphorus
The mixing of acid dihydride aluminium stirs evenly to get the conductive agent solution.
4. a kind of lithium sulfur battery anode material according to claim 1, which is characterized in that the preparation side of described adhesive
Method, comprising the following steps:
The phenol of 40-50 parts by weight, the propylene oxide mixing of 2-3 parts by weight are taken, the anhydrous of 10-14 times of mixture weight is added to
It in ethyl alcohol, stirs evenly, increasing temperature is 50-60 DEG C, and insulated and stirred 1-2 hours, 37% first of 70-75 parts by weight is added
Aldehyde stirs evenly, and is sent in 85-90 DEG C of water bath with thermostatic control, and the sodium hydroxide of 10-15 parts by weight is added, and insulated and stirred 3-4 is small
When, it discharges, filters, filter cake is washed, insulated and stirred 20-30 minutes at 60-65 DEG C, is cooled to room temperature to get described adhesive.
5. a kind of lithium sulfur battery anode material according to claim 4, which is characterized in that the concentration of the sodium hydroxide is
0.7-1mol/l。
6. a kind of preparation method of lithium sulfur battery anode material as described in claim 1, which comprises the following steps:
Sulphur is taken, is added in conductive agent solution, increasing temperature is 40-50 DEG C, and 4-6 hours ultrasonic, precipitating is washed in filtering, is done
It is sent in sintering furnace after dry, adhesive is added, increasing temperature is 170-175 DEG C, keeps the temperature 40-50 minutes, it is passed through argon gas protection,
Reducing temperature is 140-150 DEG C, and insulated and stirred 12-15 hours, discharging was cooled to room temperature to get the lithium-sulphur cell positive electrode material
Material.
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