CN106159209A - A kind of preparation method of foamy graphite alkene lithium-sulphur cell positive electrode sheet - Google Patents
A kind of preparation method of foamy graphite alkene lithium-sulphur cell positive electrode sheet Download PDFInfo
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- CN106159209A CN106159209A CN201610671807.7A CN201610671807A CN106159209A CN 106159209 A CN106159209 A CN 106159209A CN 201610671807 A CN201610671807 A CN 201610671807A CN 106159209 A CN106159209 A CN 106159209A
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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
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
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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
- H01M4/64—Carriers or collectors
- H01M4/70—Carriers or collectors characterised by shape or form
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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 the preparation method of a kind of foamy graphite alkene lithium-sulphur cell positive electrode sheet, including following step: step (1) joins ball milling 30 60min in ball mill by fine to graphite oxide and polypropylene, then the mixture after ball milling is joined ethanol and ultrasonic disperse in the mixed solution of water, forms the suspension of concentration 1 20g/L；Nickel foam is soaked 10 60min, solvent evaporated in above-mentioned suspension by step (2), places into 800 1100 DEG C of reaction 1 10h in the Muffle furnace of hydrogen nitrogen mixed gas protection, natural cooling after reaction completely；Above-mentioned product be impregnated in the hydrochloric acid of 1 3mol/L by step (3), 60 80 DEG C of reaction 5 10h, obtains foamy graphite alkene after reaction completely；Elemental sulfur powder is spread upon the surface of foamy graphite alkene by step (4), is placed in the container of sealing, and 120 180 DEG C of reaction 1 5h, after cooling, Kun pressure obtains electrode slice.Preparation method of the present invention is simple, can directly obtain lithium-sulphur cell positive electrode sheet, simplify positive pole preparation technology.
Description
Technical field
The invention belongs to lithium-sulfur cell technical field, particularly relate to the system of a kind of foamy graphite alkene lithium-sulphur cell positive electrode sheet
Preparation Method.
Background technology
Lithium-sulfur cell is with lithium metal as negative pole, and elemental sulfur is the battery system of positive pole.There are two the putting of lithium-sulfur cell
Level platform (about 2.4 V and 2.1 V), but its electrochemical reaction mechanism is more complicated.It is high that lithium-sulfur cell has specific energy
(2600 Wh/kg), specific capacity high (1675 mAh/g), low cost and other advantages are it is considered to be the most promising a new generation is electric
Pond.
But there is that active material utilization is low, cycle life is low at present and the problem such as poor stability, this seriously makes
About the development of lithium-sulfur cell.The main cause causing the problems referred to above has the following aspects: (1) elemental sulfur is electronics and ion
Insulator, room-temperature conductivity is low by (5 × 10-30S·cm-1), owing to there is no the sulfur of ionic state, thus live as positive electrode
Change difficulty；(2) the height poly-state many lithium sulfides Li produced in electrode process2Sn(8 ＞ n >=4) it is soluble in electrolyte,
Forming concentration difference between both positive and negative polarity, move to negative pole under the effect of Concentraton gradient, the high many lithium sulfides of poly-state are by lithium metal also
The many lithium sulfides of the oligomeric state of former one-tenth.Along with the carrying out of above reaction, the many lithium sulfides of oligomeric state are assembled at negative pole, finally two electrodes it
Between formed concentration difference, move to again positive pole and be oxidized to the high many lithium sulfides of poly-state.This phenomenon is referred to as shuttle effect, reduces
The utilization rate of sulfur active substance.The most insoluble Li2S and Li2S2It is deposited on cathode of lithium surface, is further degrading lithium sulfur
The performance of battery；(3) reaction end product Li2S is electronic body equally, can be deposited on sulfur electrode, and lithium ion is solid
In state lithium sulfide, migration velocity is slow, makes electrochemical reaction kinetic rate slack-off；(4) sulfur and end product Li2The density of S is not
With, after sulfur is lithiated, volumetric expansion about 79%, is easily caused Li2The efflorescence of S, causes the safety problem of lithium-sulfur cell.Above-mentioned not
Foot governs the development of lithium-sulfur cell, and this is also the Important Problems that the research of current lithium-sulfur cell needs to solve.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of a kind of foamy graphite alkene lithium-sulphur cell positive electrode sheet, its
Purpose is to improve the positive electrode capacity of lithium-sulfur cell, improves the cycle life of battery, solves tradition lithium-sulfur cell in discharge and recharge
Intermediate product polysulfide in journey is dissolved in electrolyte, makes the positive electrode capacity of lithium-sulfur cell drastically decline, causes the circulation of battery
The problem that life-span is deteriorated.
The present invention provides the preparation method of the preparation method of a kind of foamy graphite alkene lithium-sulphur cell positive electrode sheet to be:
Step (1) joins ball milling 30-60min in ball mill, then by the mixing after ball milling by fine to graphite oxide and polypropylene
Thing joins ethanol and ultrasonic disperse in the mixed solution of water, forms the suspension of concentration 1-20g/L.
Nickel foam is soaked 10-60min, solvent evaporated in above-mentioned suspension by step (2), places into hydrogen nitrogen mixed gas and protects
800-1100 DEG C of reaction 1-10h, natural cooling after reaction completely in the Muffle furnace protected.
Above-mentioned product be impregnated in the hydrochloric acid of 1-3mol/L by step (3), and 60-80 DEG C of reaction 5-10h, after reaction completely
Obtain foamy graphite alkene.
Elemental sulfur powder is spread upon the surface of foamy graphite alkene by step (4), is placed in the container of sealing, and 120-180 DEG C anti-
Answering 1-5h, after cooling, Kun pressure obtains electrode slice.
Further, in described step (1), Ball-milling Time is 30-60min；
Further, the 0.01-5% that quality is graphite oxide quality that in described step (1), polypropylene is fine.
Further, in described step (1), in the mixed solution of ethanol and water, the volume ratio of ethanol and water is 0.25-4.
Further, described step (1) is at the suspension that concentration is 1-20g/L of graphite oxide suspension.
Further, in described step (2), nickel foam is immersed in the time in graphite oxide suspension is 10-60min.
Further, in described step (2), the atmosphere in Muffle furnace is the hydrogen nitrogen mixed gas containing volumetric concentration 5% hydrogen.
Further, the described step (2) reaction temperature in Muffle furnace is 800-1100 DEG C, and the response time is 1-10h.
Further, in described step (3), concentration of hydrochloric acid is 1-3mol/L.
Further, the described step (3) reaction temperature in hydrochloric acid is 60-80 DEG C, and the response time is 5-10h.
Further, in described step (4) 0.5-5 times of the quality that quality is foamy graphite alkene of sulfur.
Further, in described step (4), reaction temperature is 120-180 DEG C, and the response time is 1-5h.
Further, the thickness of the electrode slice obtained in described step (4) is 100-500um.
There is advantages that (1) preparation method of the present invention is simple, lithium-sulphur cell positive electrode can be directly obtained
Sheet, simplifies positive pole preparation technology；(2) foamy graphite alkene not only can play support and electric action as collector but also can make
Storage sulfur space is provided for positive electrode；(3) foamy graphite alkene has bigger specific surface area and pore volume, can prepare high load sulfur content
Positive pole, can effectively suppress effect of shuttling back and forth simultaneously, improves the lithium-sulfur cell life-span.
Accompanying drawing explanation
Fig. 1 is the cycle life figure of the embodiment of the present invention 1 lithium sulphur battery electrode sheet.
Detailed description of the invention
Below in conjunction with the accompanying drawings, the preferably embodiment of the present invention is described in further detail:
Embodiment 1
(1) ball milling 30min in ball mill is joined, then by mixing after ball milling by fine to 10g graphite oxide and 0.001g polypropylene
Compound joins ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 0.25, forms the suspension of concentration 1g/L.
(2) nickel foam is soaked in above-mentioned suspension 10min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen
800 DEG C of reaction 10h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 1mol/L, 60 DEG C of reaction 10h, obtain foam stone after reaction completely
Ink alkene.
(4) 5g elemental sulfur powder is spread upon the surface of foamy graphite alkene, is placed in the container of sealing, 120 DEG C of reaction 5h,
After cooling, Kun pressure obtains electrode slice.
Embodiment 2
(1) ball milling 60min in ball mill is joined, then by the mixing after ball milling by fine to 10g graphite oxide and 0.5g polypropylene
Thing joins ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 4, forms the suspension of concentration 20g/L.
(2) nickel foam is soaked in above-mentioned suspension 60min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen
1100 DEG C of reaction 1h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 3mol/L, 80 DEG C of reaction 5h, obtain foam stone after reaction completely
Ink alkene.
(4) 50g elemental sulfur powder is spread upon the surface of foamy graphite alkene, is placed in the container of sealing, 180 DEG C of reaction 1h,
After cooling, Kun pressure obtains electrode slice.
Embodiment 3
(1) ball milling 45min in ball mill is joined, then by the mixing after ball milling by fine to 10g graphite oxide and 0.1g polypropylene
Thing joins ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 0.5, forms the suspension of concentration 3g/L.
(2) nickel foam is soaked in above-mentioned suspension 30min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen
900 DEG C of reaction 5h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 2mol/L, 75 DEG C of reaction 7h, obtain foamy graphite after reaction completely
Alkene.
(4) 10g elemental sulfur powder is spread upon the surface of foamy graphite alkene, is placed in the container of sealing, 150 DEG C of reaction 3h,
After cooling, Kun pressure obtains electrode slice.
Embodiment 4
(1) ball milling 40min in ball mill is joined, then by the mixture after ball milling by fine to 10g graphite oxide and 3g polypropylene
Join ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 2, form the suspension of concentration 10g/L.
(2) nickel foam is soaked in above-mentioned suspension 50min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen
1000 DEG C of reaction 3h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 1.5mol/L, 65 DEG C of reaction 9h, obtain foam stone after reaction completely
Ink alkene.
(4) 20g elemental sulfur powder is spread upon the surface of foamy graphite alkene, is placed in the container of sealing, 160 DEG C of reaction 2h,
After cooling, Kun pressure obtains electrode slice.
Embodiment 5
(1) ball milling 40min in ball mill is joined, then by the mixture after ball milling by fine to 10g graphite oxide and 1g polypropylene
Join ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 1, form the suspension of concentration 5g/L.
(2) nickel foam is soaked in above-mentioned suspension 20min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen
950 DEG C of reaction 80h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 2.5mol/L, 75 DEG C of reaction 4h, obtain foam stone after reaction completely
Ink alkene.
(4) 30g elemental sulfur powder is spread upon the surface of foamy graphite alkene, is placed in the container of sealing, 140 DEG C of reaction 4h,
After cooling, Kun pressure obtains electrode slice.
Its effect is as shown in table 1, as shown in Table 1: lithium sulphur battery electrode tablet quality specific capacity prepared by the present invention reaches
1290-1410 mAh/g。
As shown in Figure 1: lithium sulphur battery electrode sheet discharge and recharge prepared by the present invention 300 times, property retention is good.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Energy density (mAh/g) | 1375 | 1410 | 1290 | 1345 | 1336 |
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert this
Bright being embodied as is confined to these explanations.For general technical staff of the technical field of the invention, do not taking off
On the premise of present inventive concept, it is also possible to make some simple deduction or replace, all should be considered as belonging to the protection of the present invention
Scope.
Claims (10)
1. the preparation method of a foamy graphite alkene lithium-sulphur cell positive electrode sheet, it is characterised in that include following step:
Step (1) joins ball milling 30-60min in ball mill, then by the mixing after ball milling by fine to graphite oxide and polypropylene
Thing joins ethanol and ultrasonic disperse in the mixed solution of water, forms the suspension of concentration 1-20g/L；
Nickel foam is soaked 10-60min, solvent evaporated in above-mentioned suspension by step (2), places into hydrogen nitrogen mixed gas protection
800-1100 DEG C of reaction 1-10h, natural cooling after reaction completely in Muffle furnace；
Above-mentioned product be impregnated in the hydrochloric acid of 1-3mol/L by step (3), 60-80 DEG C of reaction 5-10h, obtains after reaction completely
Foamy graphite alkene；
Elemental sulfur powder is spread upon the surface of foamy graphite alkene by step (4), is placed in the container of sealing, 120-180 DEG C of reaction 1-
5h, after cooling, Kun pressure obtains electrode slice.
2. preparation method as claimed in claim 1, it is characterised in that in described step (1), Ball-milling Time is 30-60min.
3. preparation method as claimed in claim 1, it is characterised in that the quality that in described step (1), polypropylene is fine is oxidation
The 0.01-5% of graphite quality.
4. preparation method as claimed in claim 1, it is characterised in that in described step (1) in the mixed solution of ethanol and water
Ethanol is 0.25-4 with the volume ratio of water.
5. preparation method as claimed in claim 1, it is characterised in that described step (1) is in the concentration of graphite oxide suspension
Suspension for 1-20g/L.
6. preparation method as claimed in claim 1, it is characterised in that in described step (2), nickel foam is immersed in graphite oxide
Time in suspension is 10-60min.
7. preparation method as claimed in claim 1, it is characterised in that in described step (2), the atmosphere in Muffle furnace is containing body
The hydrogen nitrogen mixed gas of volume concentrations 5% hydrogen；The described step (2) reaction temperature in Muffle furnace is 800-1100 DEG C, the response time
For 1-10h.
8. preparation method as claimed in claim 1, it is characterised in that in described step (3), concentration of hydrochloric acid is 1-3mol/L；?
Reaction temperature in hydrochloric acid is 60-80 DEG C, and the response time is 5-10h.
9. preparation method as claimed in claim 1, it is characterised in that in described step (4), the quality of sulfur is foamy graphite alkene
0.5-5 times of quality.
10. preparation method as claimed in claim 1, it is characterised in that in described step (4), reaction temperature is 120-180 DEG C,
Response time is 1-5h；In the thickness of electrode slice that obtains be 100-500um.
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Cited By (5)
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| WO2018032321A1 (en) * | 2016-08-16 | 2018-02-22 | 肖丽芳 | Method for manufacturing graphene foam positive electrode for lithium-sulfur battery |
| CN107959045A (en) * | 2017-10-25 | 2018-04-24 | 西交利物浦大学 | The foamy graphite alkene piece of the porous carbon nano rod of N doping is the lithium-sulfur cell in intermediate layer |
| CN108717968A (en) * | 2018-04-27 | 2018-10-30 | 西安理工大学 | A kind of binder free anode piece preparation method for lithium-sulfur cell |
| CN108878835A (en) * | 2018-06-28 | 2018-11-23 | 肇庆市华师大光电产业研究院 | A kind of preparation method of lithium sulfur battery anode material |
| CN109524672A (en) * | 2018-11-19 | 2019-03-26 | 肇庆市华师大光电产业研究院 | A kind of mesh structural porous self-supporting flexible electrode material of three-dimensional selenium/grapheme foam, preparation method and application |
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| CN108717968B (en) * | 2018-04-27 | 2021-05-25 | 西安理工大学 | Preparation method of binder-free positive plate for lithium-sulfur battery |
| CN108878835A (en) * | 2018-06-28 | 2018-11-23 | 肇庆市华师大光电产业研究院 | A kind of preparation method of lithium sulfur battery anode material |
| CN109524672A (en) * | 2018-11-19 | 2019-03-26 | 肇庆市华师大光电产业研究院 | A kind of mesh structural porous self-supporting flexible electrode material of three-dimensional selenium/grapheme foam, preparation method and application |
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