CN107104230A - A kind of preparation method of high-energy density lithium sulphur battery material - Google Patents
A kind of preparation method of high-energy density lithium sulphur battery material Download PDFInfo
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- CN107104230A CN107104230A CN201710476823.5A CN201710476823A CN107104230A CN 107104230 A CN107104230 A CN 107104230A CN 201710476823 A CN201710476823 A CN 201710476823A CN 107104230 A CN107104230 A CN 107104230A
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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
- H01M4/366—Composites as layered products
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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
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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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- 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 preparation method of high-energy density lithium sulphur battery material, methods described prepares nano-sulfur using sulfuric acid and sodium thiosulfate reaction, by silicon dioxide coated nano sulphur and prepares microballoon, improves the cycle performance of lithium-sulfur cell；The present invention is coated using the stratum level hole carbon material of three-dimensional structure, active component capacity is improved with meso-hole structure, and three-dimensional structure can effectively improve the scattering and permeating of electrolyte, electronic and ionic efficiency of transmission is improved, circulation and the high rate performance of positive electrode is effectively improved.
Description
Technical field
The present invention relates to battery material field, and in particular to a kind of preparation method of high-energy density lithium sulphur battery material.
Background technology
New energy industry is that the current whole world improves an important development direction of energy shortage and environmental protection.Lithium-ion electric
Pond is due to high operating voltage, and memory-less effect, self discharge is small, energy density is big and the advantage that has extended cycle life, by
To extensive concern.Current lithium ion battery mainly develops towards high-energy-density, low production cost, high safety direction.
By negative pole of lithium metal, elemental sulfur for the theoretical specific energy of the lithium-sulfur cell of positive pole can reach 2600Wh/kg (lithium and
The theoretical specific capacity of sulphur is respectively 3860mAh/g and 1675mAh/g), much larger than used commercialization secondary cell at this stage.
In addition, cheap, the environment-friendly characteristic of elemental sulfur makes the energy storage system great commercial value again.But in the prior art, lithium
Not high to the utilization rate of positive active material sulphur in sulphur battery, its Capacity fading is serious, and cycle performance is poor, and electrochemistry
Performance is not good.In order to improve the performance of lithium-sulfur cell, current people are directed to the research of the positive electrode modification to lithium-sulfur cell,
To improve its electric conductivity and cycle performance.For example sulphur is filled out in mesoporous carbon space, the addition of mesoporous carbon improves electric conductivity；This
There is research worker to be modified using conducting polymer to sulphur outside, the addition of conducting polymer can be effectively improved lithium sulphur electricity
The cycle performance in pond.Although however, above-mentioned can improve the electric conductivity of lithium-sulfur cell to the method that sulphur positive electrode is modified
Or its cycle performance is improved, but the energy density of obtained lithium-sulfur cell is reduced, that is to say, that it is this that sulphur positive electrode is entered
The modified method of row can not improve the performance of lithium-sulfur cell on the whole.
In order to overcome above mentioned problem, the performance of lithium-sulfur cell is lifted, people are by elemental sulfur and various micropore/mesoporous carbon materials
It is compound with conducting polymer materials, to strengthen the electrical conductance of elemental sulfur, while suppressing the dissolving of polysulfide；Or using conductive
Polymer overmold is to reach above-mentioned purpose；Or inorganic oxide is added in anode composite material as many sulphur of adsorbent absorption
Compound is in positive pole.By years of researches, the specific capacity and cycle performance of lithium-sulfur cell have very big lifting.
The content of the invention
The present invention provides a kind of preparation method of high-energy density lithium sulphur battery material, methods described using sulfuric acid with it is thio
Sodium sulphate reaction prepares nano-sulfur, by silicon dioxide coated nano sulphur and prepares microballoon, improves the cyclicity of lithium-sulfur cell
Energy；The present invention is coated using the stratum level hole carbon material of three-dimensional structure, and active component capacity is improved with meso-hole structure,
And three-dimensional structure can effectively improve the scattering and permeating of electrolyte, electronic and ionic efficiency of transmission is improved, positive pole material is effectively improved
The circulation of material and high rate performance.
To achieve these goals, the present invention provides a kind of preparation method of high-energy density lithium sulphur battery material, the party
Method comprises the following steps：
（1）Prepare silica nanometer sulphur
Count by weight, the 35-40 parts of poly-vinyl alcohol solutions of mass fraction 5%, 10-12 parts of sodium thiosulfate and 12- are weighed respectively
15 parts of 10mol/L sulfuric acid are placed in beaker, and stirring mixing is placed in ultrasonic disperse 10-15min under 300-400W, then stands old
Change 4-6h, filter cake is collected by filtration and with water washing is distilled 3-5 times, filter cake must be washed by collecting, and be counted by weight, be weighed respectively
45-50 parts of distilled water, 10-15 parts without water glycol, 4-6 parts of polyvinyl alcohol and 6-8 parts of washing filter cakes, it is ultrasonic under 300-400W
Scattered 10-15min, is prepared into modified dispersion liquid；
The modification dispersion liquid pH to 10-11 for choosing the above-mentioned preparation of the ammoniacal liquor of mass fraction 12% regulation is placed in conical flask, is collected
Obtain alkalization modified liquid, then in mass ratio 1:8, the tetraethyl orthosilicate ethylene glycol solution of mass fraction 7% is added dropwise in conical beaker,
It is 80-100min to control time for adding, after being added dropwise to complete, sealing reaction 3-5h, then filters and collects filter cake, uses anhydrous second
After glycol is washed 3-5 times, 5-6h is dried at 50-60 DEG C, silica nanometer sulphur is prepared；
（2）Prepare three-dimensional flower-shaped carbon material
Potassium hydroxide and zinc acetate progress hydro-thermal reaction soluble in water are obtained to the matter of flower shape zinc oxide, potassium hydroxide and zinc acetate
Amount is than being 3:(2-4)；
Flower shape zinc oxide, mesoporous pore creating material are mixed in water into then addition trishydroxymethylaminomethane and dopamine sulfate to enter
Row mixing coating reaction, product suction filtration is then dried, solid product is obtained in one layer of meso-hole structure of flower shape zinc oxide surface construction
One, the flower shape zinc oxide, mesoporous pore creating material, the mass ratio of trishydroxymethylaminomethane and dopamine sulfate are 10:(3-
5):(2-3):(2-4)；
Gained solid product one, micropore pore creating material dodecyl sulphate potassium are uniformly mixed in water, three hydroxyls are then sequentially added
Aminomethane and dopamine sulfate carry out mixing coating reaction, on the basis of the meso-hole structure that solid product one is constructed
One layer of microcellular structure is coated, solid product two is obtained；Then suction filtration, drying, carbonization are carried out, then zinc oxide template is removed with acid, is obtained
Three-dimensional flower-shaped carbon material with micropore, meso-hole structure；The solid product one, micropore pore creating material dodecyl sulphate potassium, three
The mass ratio of hydroxymethyl aminomethane and dopamine sulfate is 10:(1-2):(4-5):(9-11)；
（3）Compound coating
The three-dimensional flower-shaped carbon material of gained and the silica nanometer sulfur materials are combined, compound condition is：In nitrogen bar
Under part, 150-200 DEG C is heated to, 20-24h is incubated, is then purged, the silica nanometer sulphur being not filled by into duct is removed
Material, obtains three-dimensional carbon composite sulfur lithium anode material.
It is preferred that, the step（2）In, hydrothermal temperature is 80-90 DEG C, and the reaction time is 30-50min, described mixed
The temperature for closing coating reaction is 25-40 DEG C, and the time is 6-8h.
The invention has the advantages that and remarkable result：
（1）The present invention prepares nano-sulfur using sulfuric acid and sodium thiosulfate reaction, by silicon dioxide coated nano sulphur and prepares
Microballoon, improves the cycle performance of lithium-sulfur cell.
（2）The present invention is coated using the stratum level hole carbon material of three-dimensional structure, and activity is improved with meso-hole structure
Composition capacity, and three-dimensional structure can effectively improve the scattering and permeating of electrolyte, improve electronic and ionic efficiency of transmission, be effectively improved
The circulation of positive electrode and high rate performance.
Embodiment
Embodiment one
Count by weight, respectively 35 parts of poly-vinyl alcohol solutions of mass fraction 5% of weighing, 10 parts of sodium thiosulfate and 12 parts
10mol/L sulfuric acid is placed in beaker, and stirring mixing is placed in ultrasonic disperse 10min under 300W, and subsequent still aging 4h, filtering is received
Collect filter cake and with water washing is distilled 3 times, filter cake must be washed by collecting, and be counted by weight, and 45 parts of distilled water, 10 parts of nothings are weighed respectively
Water glycol, 4 parts of polyvinyl alcohol and 6 parts of washing filter cakes, the ultrasonic disperse 10min under 300W are prepared into modified dispersion liquid；
The modification dispersion liquid pH to 10-11 for choosing the above-mentioned preparation of the ammoniacal liquor of mass fraction 12% regulation is placed in conical flask, is collected
Obtain alkalization modified liquid, then in mass ratio 1:8, the tetraethyl orthosilicate ethylene glycol solution of mass fraction 7% is added dropwise in conical beaker,
It is 80min to control time for adding, after being added dropwise to complete, sealing reaction 3h, then filters and collects filter cake, is washed with without water glycol
Wash after 3 times, 5h is dried at 50 DEG C, silica nanometer sulphur is prepared.
Potassium hydroxide and the zinc acetate hydro-thermal reaction soluble in water that carries out are obtained into flower shape zinc oxide, potassium hydroxide and zinc acetate
Mass ratio be 3:2；Hydrothermal temperature is 80 DEG C, and the reaction time is 30min.
Flower shape zinc oxide, mesoporous pore creating material are mixed in water and then added trishydroxymethylaminomethane and dopamine sulfuric acid
Salt carries out mixing coating reaction, then dries product suction filtration, solid is obtained in one layer of meso-hole structure of flower shape zinc oxide surface construction
Product one, the flower shape zinc oxide, mesoporous pore creating material, the mass ratio of trishydroxymethylaminomethane and dopamine sulfate are 10:
3:2:2；The temperature of the mixing coating reaction is 25 DEG C, and the time is 6h.
Gained solid product one, micropore pore creating material dodecyl sulphate potassium are uniformly mixed in water, then sequentially added
Trishydroxymethylaminomethane and dopamine sulfate carry out mixing coating reaction, the base for the meso-hole structure constructed in solid product one
One layer of microcellular structure is coated on plinth, solid product two is obtained；Then suction filtration, drying, carbonization are carried out, then zinc oxide mould is removed with acid
Plate, obtains the three-dimensional flower-shaped carbon material with micropore, meso-hole structure；The solid product one, micropore pore creating material dodecyl sulphate
The mass ratio of potassium, trishydroxymethylaminomethane and dopamine sulfate is 10:1:4:9.
The three-dimensional flower-shaped carbon material of gained and the silica nanometer sulfur materials are combined, compound condition is：In nitrogen
Under the conditions of gas, 150 DEG C are heated to, 20h is incubated, is then purged, the silica nanometer sulphur material being not filled by into duct is removed
Material, obtains three-dimensional carbon composite sulfur lithium anode material.
Embodiment two
Count by weight, respectively 40 parts of poly-vinyl alcohol solutions of mass fraction 5% of weighing, 12 parts of sodium thiosulfate and 15 parts
10mol/L sulfuric acid is placed in beaker, and stirring mixing is placed in ultrasonic disperse 15min under 400W, and subsequent still aging 6h, filtering is received
Collect filter cake and with water washing is distilled 5 times, filter cake must be washed by collecting, and be counted by weight, and 50 parts of distilled water, 15 parts of nothings are weighed respectively
Water glycol, 6 parts of polyvinyl alcohol and 8 parts of washing filter cakes, the ultrasonic disperse 15min under 400W are prepared into modified dispersion liquid；
The modification dispersion liquid pH to 10-11 for choosing the above-mentioned preparation of the ammoniacal liquor of mass fraction 12% regulation is placed in conical flask, is collected
Obtain alkalization modified liquid, then in mass ratio 1:8, the tetraethyl orthosilicate ethylene glycol solution of mass fraction 7% is added dropwise in conical beaker,
It is 100min to control time for adding, after being added dropwise to complete, sealing reaction 5h, then filters and collects filter cake, with without water glycol
After washing 5 times, 6h is dried at 60 DEG C, silica nanometer sulphur is prepared.
Potassium hydroxide and the zinc acetate hydro-thermal reaction soluble in water that carries out are obtained into flower shape zinc oxide, potassium hydroxide and zinc acetate
Mass ratio be 3:4；Hydrothermal temperature is 90 DEG C, and the reaction time is 50min.
Flower shape zinc oxide, mesoporous pore creating material are mixed in water and then added trishydroxymethylaminomethane and dopamine sulfuric acid
Salt carries out mixing coating reaction, then dries product suction filtration, solid is obtained in one layer of meso-hole structure of flower shape zinc oxide surface construction
Product one, the flower shape zinc oxide, mesoporous pore creating material, the mass ratio of trishydroxymethylaminomethane and dopamine sulfate are 10:
5:3:4；The temperature of the mixing coating reaction is 40 DEG C, and the time is 8h.
Gained solid product one, micropore pore creating material dodecyl sulphate potassium are uniformly mixed in water, then sequentially added
Trishydroxymethylaminomethane and dopamine sulfate carry out mixing coating reaction, the base for the meso-hole structure constructed in solid product one
One layer of microcellular structure is coated on plinth, solid product two is obtained；Then suction filtration, drying, carbonization are carried out, then zinc oxide mould is removed with acid
Plate, obtains the three-dimensional flower-shaped carbon material with micropore, meso-hole structure；The solid product one, micropore pore creating material dodecyl sulphate
The mass ratio of potassium, trishydroxymethylaminomethane and dopamine sulfate is 10:2:5:11.
The three-dimensional flower-shaped carbon material of gained and the silica nanometer sulfur materials are combined, compound condition is：In nitrogen
Under the conditions of gas, 200 DEG C are heated to, 24h is incubated, is then purged, the silica nanometer sulphur material being not filled by into duct is removed
Material, obtains three-dimensional carbon composite sulfur lithium anode material.
Comparative example
Commercially available sulphur lithium anode material.
Above-described embodiment one, two and comparative example products therefrom are used into NMP as solvent, by active material: SP: PVDF
Be configured to slurry that solid content be 70% at=90: 5: 5 is evenly applied on Al paper tinsels, and positive pole is made.Negative pole is from diameter 14mm's
Metal lithium sheet, electrolyte selects 1mol LiFP6 (EC：DMC：EMC=1:1:1, v/v), with negative electrode casing-shell fragment-pad-lithium
Battery is packaged by the order of piece-electrolyte-barrier film-positive plate-pad-anode cover, and whole process is all filled with argon
Completed in the glove box of gas.Electric performance test is carried out in the case where test temperature is 25 DEG C, after tested the material of the embodiment one and two
Compared with the product of comparative example, first charge-discharge reversible capacity improves 15-20%, and service life brings up to more than 15%.
Claims (2)
1. a kind of preparation method of high-energy density lithium sulphur battery material, this method comprises the following steps：
（1）Prepare silica nanometer sulphur
Count by weight, the 35-40 parts of poly-vinyl alcohol solutions of mass fraction 5%, 10-12 parts of sodium thiosulfate and 12- are weighed respectively
15 parts of 10mol/L sulfuric acid are placed in beaker, and stirring mixing is placed in ultrasonic disperse 10-15min under 300-400W, then stands old
Change 4-6h, filter cake is collected by filtration and with water washing is distilled 3-5 times, filter cake must be washed by collecting, and be counted by weight, be weighed respectively
45-50 parts of distilled water, 10-15 parts without water glycol, 4-6 parts of polyvinyl alcohol and 6-8 parts of washing filter cakes, it is ultrasonic under 300-400W
Scattered 10-15min, is prepared into modified dispersion liquid；
The modification dispersion liquid pH to 10-11 for choosing the above-mentioned preparation of the ammoniacal liquor of mass fraction 12% regulation is placed in conical flask, is collected
Obtain alkalization modified liquid, then in mass ratio 1:8, the tetraethyl orthosilicate ethylene glycol solution of mass fraction 7% is added dropwise in conical beaker,
It is 80-100min to control time for adding, after being added dropwise to complete, sealing reaction 3-5h, then filters and collects filter cake, uses anhydrous second
After glycol is washed 3-5 times, 5-6h is dried at 50-60 DEG C, silica nanometer sulphur is prepared；
（2）Prepare three-dimensional flower-shaped carbon material
Potassium hydroxide and zinc acetate progress hydro-thermal reaction soluble in water are obtained to the matter of flower shape zinc oxide, potassium hydroxide and zinc acetate
Amount is than being 3:(2-4)；
Flower shape zinc oxide, mesoporous pore creating material are mixed in water into then addition trishydroxymethylaminomethane and dopamine sulfate to enter
Row mixing coating reaction, product suction filtration is then dried, solid product is obtained in one layer of meso-hole structure of flower shape zinc oxide surface construction
One, the flower shape zinc oxide, mesoporous pore creating material, the mass ratio of trishydroxymethylaminomethane and dopamine sulfate are 10:(3-
5):(2-3):(2-4)；
Gained solid product one, micropore pore creating material dodecyl sulphate potassium are uniformly mixed in water, three hydroxyls are then sequentially added
Aminomethane and dopamine sulfate carry out mixing coating reaction, on the basis of the meso-hole structure that solid product one is constructed
One layer of microcellular structure is coated, solid product two is obtained；Then suction filtration, drying, carbonization are carried out, then zinc oxide template is removed with acid, is obtained
Three-dimensional flower-shaped carbon material with micropore, meso-hole structure；The solid product one, micropore pore creating material dodecyl sulphate potassium, three
The mass ratio of hydroxymethyl aminomethane and dopamine sulfate is 10:(1-2):(4-5):(9-11)；
（3）Compound coating
The three-dimensional flower-shaped carbon material of gained and the silica nanometer sulfur materials are combined, compound condition is：In nitrogen bar
Under part, 150-200 DEG C is heated to, 20-24h is incubated, is then purged, the silica nanometer sulphur being not filled by into duct is removed
Material, obtains three-dimensional carbon composite sulfur lithium anode material.
2. the method as described in claim 1, it is characterised in that the step（2）In, hydrothermal temperature is 80-90 DEG C, instead
It is 30-50min between seasonable, the temperature of the mixing coating reaction is 25-40 DEG C, and the time is 6-8h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104118901A (en) * | 2014-07-23 | 2014-10-29 | 西安工程大学 | Preparation method of flower-like nano zinc oxide |
| CN106654231A (en) * | 2017-01-23 | 2017-05-10 | 武汉理工大学 | Anode material for lithium sulfur batteries and method for preparing anode material |
| CN106784637A (en) * | 2016-12-30 | 2017-05-31 | 梅庆波 | A kind of preparation method of high-energy-density lithium-sulphur cell positive electrode material |
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2017
- 2017-06-21 CN CN201710476823.5A patent/CN107104230A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104118901A (en) * | 2014-07-23 | 2014-10-29 | 西安工程大学 | Preparation method of flower-like nano zinc oxide |
| CN106784637A (en) * | 2016-12-30 | 2017-05-31 | 梅庆波 | A kind of preparation method of high-energy-density lithium-sulphur cell positive electrode material |
| CN106654231A (en) * | 2017-01-23 | 2017-05-10 | 武汉理工大学 | Anode material for lithium sulfur batteries and method for preparing anode material |
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Application publication date: 20170829 |