CN106207097A - A kind of lithium-sulfur cell pole piece and the preparation method of battery thereof - Google Patents
A kind of lithium-sulfur cell pole piece and the preparation method of battery thereof Download PDFInfo
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- CN106207097A CN106207097A CN201610616049.9A CN201610616049A CN106207097A CN 106207097 A CN106207097 A CN 106207097A CN 201610616049 A CN201610616049 A CN 201610616049A CN 106207097 A CN106207097 A CN 106207097A
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- H—ELECTRICITY
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention provides a kind of lithium-sulfur cell pole piece and the preparation method of battery thereof, including lithium anode, sulfur positive plate and barrier film；Described sulfur positive plate includes collector and is positioned at the first sulfur carbon composite coated layer being sequentially distributed thereon, for stopping the second sulfur carbon composite coated layer of sulfur loss in the first sulfur carbon composite coated layer and for stopping the 3rd composite coated layer that in the first sulfur carbon composite coated layer, sulfur runs off.The present invention uses this structure, can be effectively increased positive plate ionic conductivity and electronic conductivity effectively by the sulfur active material in the first coat within lithium ion conduction cause.
Description
Technical field
The invention belongs to lithium-sulfur cell technical field, particularly relate to the preparation method of a kind of lithium-sulphur cell positive electrode sheet.
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 governs lithium
The development of sulfur battery.The main cause causing the problems referred to above has the following aspects: (1) elemental sulfur is electronics and ion insulation
Body, room-temperature conductivity is low by (5 × 10-30S·cm-1), owing to there is no the sulfur of ionic state, thus tired as positive electrode activation
Difficult；(2) the height poly-state many lithium sulfides Li produced in electrode process2Sn(8 ＞ n >=4) it is soluble in electrolyte, just
Forming concentration difference between negative pole, move to negative pole under the effect of Concentraton gradient, the high many lithium sulfides of poly-state are reduced into by lithium metal
The many lithium sulfides of oligomeric state.Along with the carrying out of above reaction, the many lithium sulfides of oligomeric state are assembled at negative pole, shape the most between electrodes
Become 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 sulfur and lives
The utilization rate of property material.The most insoluble Li2S and Li2S2It is deposited on cathode of lithium surface, is further degrading lithium-sulfur cell
Performance；(3) reaction end product Li2S is electronic body equally, can be deposited on sulfur electrode, and lithium ion is at solid-state sulfur
Change migration velocity in lithium slow, make electrochemical reaction kinetic rate slack-off；(4) sulfur and end product Li2The density of S is different, when
Sulfur is lithiated rear volumetric expansion about 79%, is easily caused Li2The efflorescence of S, causes the safety problem of lithium-sulfur cell.Above-mentioned not enough system
About the development of lithium-sulfur cell, this be also current lithium-sulfur cell research need solve Important Problems.
For improving specific discharge capacity and the cycle life of lithium-sulfur cell, disclose at present and put between lithium-sulfur cell both positive and negative polarity
Put independent carbon film interlayer, will material with carbon element and the mixing of PTFE binding agent roll-in film forming, or use the material such as carbon cloth
Material, forms the independent carbon film with self-supporting ability, this carbon film not only complicated process of preparation, and thickness big, and weight is high, lithium sulfur
Battery assembling process difficulty is big, reduces performance and the application potential of lithium-sulfur cell.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of lithium-sulphur cell positive electrode and the battery comprising this positive pole, its purpose
It is to improve the positive electrode capacity of lithium-sulfur cell, improves the cycle life of battery, solve tradition lithium-sulfur cell in charge and discharge process
Intermediate product polysulfide be dissolved in electrolyte, make the positive electrode capacity of lithium-sulfur cell drastically decline, cause the cycle life of battery
The problem being deteriorated.
A kind of lithium-sulfur cell, including lithium anode, sulfur positive plate and barrier film；
Wherein sulfur positive plate feature is: includes collector and is positioned at the first sulfur carbon composite coated layer thereon, and the second sulfur carbon is combined
Coat, the 3rd composite coated layer, it also includes for stopping the second sulfur carbon that in the first sulfur carbon composite coated layer, sulfur runs off multiple
Closing coat, it is positioned on the first sulfur carbon composite coated layer, and it also includes for stopping sulfur stream in the second sulfur carbon composite coated layer
The 3rd composite coated layer lost, it is positioned on the second sulfur carbon composite coated layer.
Further, the sulfur carbon mass ratio in described second sulfur carbon coat is less than the sulfur in the first sulfur carbon composite coated layer
Carbon mass ratio.
Further, the mass content of the sulfur in described first sulfur carbon coat is 50-99%, described second sulfur carbon coating
The mass content of the sulfur in Ceng is 1-50%.
Further, described second sulfur carbon coat includes Graphene, binding agent and sulfur active material.
Further, described second sulfur carbon coat Graphene has central hole structure, and its aperture is at 5-50nm.
Further, described 3rd composite coated layer includes lithium titanate, Graphene and binding agent.
Further, the first sulfur carbon coat: the second sulfur carbon coat: the thickness of the 3rd composite coated layer is than for 100:2-
5:5-10。
The present invention provides a kind of lithium sulphur battery electrode sheet and battery preparation technique flow process thereof as follows:
(1) sulfur active material, conductive agent, binding agent are joined in NMP mixed according to the ratio of weight ratio 80-90:5-10:5-10
Synthetic slurry, is then coated with on plus plate current-collecting body aluminium foil, obtains containing the first sulfur carbon coat positive plate after drying.
(2) sulfur active material, Graphene, binding agent are joined according to the ratio of weight ratio 10-40:40-80:5-10
NMP is mixed into slurry, is then coated with on the first sulfur carbon coat positive plate, obtains after drying containing the second sulfur carbon coat
Positive plate.
(3) lithium titanate material, Graphene, binding agent are joined NMP according to the ratio of weight ratio 80-90:5-10:5-10
In be mixed into slurry, be then coated with on the second sulfur carbon coat positive plate, after drying, obtain positive plate.
(4) positive plate of negative pole lithium sheet, barrier film and the present invention sticked together insert in CR2032 type button cell shell,
Injecting electrolyte in battery case, the electrolyte of injection is the DOL-DME solution (body of DOL and DME of 1mol/L LiTFSI
Long-pending ratio is 1:1), seal, obtain CR2032 type button lithium-sulfur cell.
There is advantages that (1) in order to play the effect on barrier layer, its specific implementation be lithium sulfur electricity
First, second coat of pond positive pole have employed preferably sulfur carbon mass ratio so that the sulfur carbonaceous amount in the second sulfur carbon coat
Ratio is less than the sulfur carbon mass ratio in the first sulfur carbon composite coated layer, and the more carbon in the second sulfur carbon coat is to this layer and first
Sulfur in coat serves effect of contraction, and the 3rd composite coated layer serves constraint to the sulfur in this layer first and second coat
Effect stops that the polysulfide that the reduction of sulfur simple substance generates is dissolved in electrolyte, reaches to improve the purpose of cell positive pole chip architecture；(2)
In second coat, grapheme material has the electrical conductivity of superelevation and abundant central hole structure, can be effectively by lithium ion conduction
In the sulfur active material in the first coat within Zhiing, it is effectively increased positive plate ionic conductivity and electronic conductivity；(3)
In 3rd composite coated layer, lithium titanate material is also provided that battery capacity in addition to the dissolving of constraint polysulfide；(4) the 3rd is multiple
Close lithium titanate material in coat and there is in charge and discharge process zero deformation behavior, maintain stablizing of the 3rd composite coated layer,
Be conducive to the prolongation of battery life；In (5) second coats, grapheme material has the electrical conductivity of superelevation and abundant mesopore
Structure, can be effectively increased positive plate effectively by the sulfur active material in the first coat within lithium ion conduction cause
Ionic conductivity and electronic conductivity.
Accompanying drawing explanation
Fig. 1 is lithium-sulphur cell positive electrode chip architecture schematic diagram of the present invention；
In figure, 1 collector, 2 first sulfur carbon coats, 3 second sulfur carbon coats, 4 the 3rd composite coated layers.
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
As it is shown in figure 1, described battery preparation method is:
(1) sulfur active material, acetylene black, PVDF binding agent are joined in NMP according to the ratio of weight ratio 90:5:5 it is mixed into
Slurry, is then coated with on plus plate current-collecting body 1 aluminium foil, obtains containing the first sulfur carbon coat 2 positive plate after drying.
(2) sulfur active material, Graphene, PVDF binding agent are joined in NMP according to the ratio of weight ratio 10:80:10
It is mixed into slurry, is then coated with on the first sulfur carbon coat 2 positive plate, containing the second sulfur carbon coat 2 just obtains after drying
Pole piece.
(3) lithium titanate material, Graphene, PVDF binding agent are joined in NMP mixed according to the ratio of weight ratio 90:5:5
Synthetic slurry, is then coated with on the second sulfur carbon coat 3 positive plate, forms the 3rd after drying on the second sulfur carbon coat 3
Composite coated layer 4, obtains lithium-sulphur cell positive electrode sheet.
(4) negative pole lithium sheet, barrier film and positive plate are sticked together insert in CR2032 type button cell shell, at battery case
Interior injection electrolyte, the electrolyte of injection be 1mol/L LiTFSI DOL-DME solution (volume ratio of DOL and DME is 1:
1), seal, obtain CR2032 type button lithium-sulfur cell.
Embodiment 2
(1) sulfur active material, Graphene, PVDF binding agent are joined mixing in NMP according to the ratio of weight ratio 80:10:10
Form slurry, is then coated with on plus plate current-collecting body 1 aluminium foil, obtains containing the first sulfur carbon coat 2 positive plate after drying.
(2) sulfur active material, Graphene, PVDF binding agent are joined in NMP mixed according to the ratio of weight ratio 40:55:5
Synthetic slurry, is then coated with on the first sulfur carbon coat 2 positive plate, obtains containing the second sulfur carbon coat 3 positive pole after drying
Sheet.
(3) lithium titanate material, Graphene, PVDF binding agent are joined in NMP according to the ratio of weight ratio 80:10:10
It is mixed into slurry, is then coated with on the second sulfur carbon coat 2 positive plate, on the second sulfur carbon coat 3, after drying, form the
Three composite coated layers 4, obtain lithium-sulphur cell positive electrode sheet.
(4) negative pole lithium sheet, barrier film and positive plate are sticked together insert in CR2032 type button cell shell, at battery case
Interior injection electrolyte, the electrolyte of injection be 1mol/L LiTFSI DOL-DME solution (volume ratio of DOL and DME is 1:
1), seal, obtain CR2032 type button lithium-sulfur cell.
Embodiment 3
(1) sulfur active material, acetylene black, PVDF binding agent are joined in NMP according to the ratio of weight ratio 85:8:7 it is mixed into
Slurry, is then coated with on plus plate current-collecting body 1 aluminium foil, obtains containing the first sulfur carbon coat 2 positive plate after drying.
(2) sulfur active material, Graphene, PVDF binding agent are joined mixing pulping in NMP according to the ratio of 20:73:7
Material, is then coated with on the first sulfur carbon coat 2 positive plate, obtains containing the second sulfur carbon coat 3 positive plate after drying.
(3) lithium titanate material, Graphene, PVDF binding agent are joined in NMP mixed according to the ratio of weight ratio 85:8:7
Synthetic slurry, is then coated with on the second sulfur carbon coat 3 positive plate, forms the 3rd after drying on the second sulfur carbon coat 3
Composite coated layer 4, obtains lithium-sulphur cell positive electrode sheet.
(4) negative pole lithium sheet, barrier film and positive plate are sticked together insert in CR2032 type button cell shell, at battery case
Interior injection electrolyte, the electrolyte of injection be 1mol/L LiTFSI DOL-DME solution (volume ratio of DOL and DME is 1:
1), seal, obtain CR2032 type button lithium-sulfur cell.
Embodiment 4
(1) sulfur active material, acetylene black, PVDF binding agent are joined in NMP according to the ratio of weight ratio 88:6:6 it is mixed into
Slurry, is then coated with on plus plate current-collecting body 1 aluminium foil, obtains containing the first sulfur carbon coat 2 positive plate after drying.
(2) sulfur active material, Graphene, PVDF binding agent are joined in NMP mixed according to the ratio of weight ratio 30:64:6
Synthetic slurry, is then coated with on the first sulfur carbon coat 2 positive plate, obtains containing the second sulfur carbon coat 2 positive pole after drying
Sheet.
(3) lithium titanate material, Graphene, PVDF binding agent are joined in NMP mixed according to the ratio of weight ratio 88:6:6
Synthetic slurry, is then coated with on the second sulfur carbon coat 3 positive plate, forms the 3rd after drying on the second sulfur carbon coat 3
Composite coated layer 4, obtains lithium-sulphur cell positive electrode sheet.
(4) negative pole lithium sheet, barrier film and positive plate are sticked together insert in CR2032 type button cell shell, at battery case
Interior injection electrolyte, the electrolyte of injection be 1mol/L LiTFSI DOL-DME solution (volume ratio of DOL and DME is 1:
1), seal, obtain CR2032 type button lithium-sulfur cell.
Embodiment 5
(1) sulfur active material, Graphene, PVDF binding agent are joined in NMP according to the ratio of weight ratio 82:9:9 it is mixed into
Slurry, is then coated with on plus plate current-collecting body 1 aluminium foil, obtains containing the first sulfur carbon coat 2 positive plate after drying.
(2) sulfur active material, Graphene, PVDF binding agent are joined in NMP mixed according to the ratio of weight ratio 25:70:5
Synthetic slurry, is then coated with on the first sulfur carbon coat 2 positive plate, obtains containing the second sulfur carbon coat 3 positive pole after drying
Sheet.
(3) lithium titanate material, Graphene, PVDF binding agent are joined in NMP mixed according to the ratio of weight ratio 82:9:9
Synthetic slurry, is then coated with on the second sulfur carbon coat 3 positive plate, forms the 3rd after drying on the second sulfur carbon coat 3
Composite coated layer 4, obtains lithium-sulphur cell positive electrode sheet.
(4) negative pole lithium sheet, barrier film and positive plate are sticked together insert in CR2032 type button cell shell, at battery case
Interior injection electrolyte, the electrolyte of injection be 1mol/L LiTFSI DOL-DME solution (volume ratio of DOL and DME is 1:
1), seal, obtain CR2032 type button lithium-sulfur cell.
Comparative example 1
(1) sulfur active material, acetylene black, PVDF binding agent are joined in NMP according to the ratio of weight ratio 90:5:5 it is mixed into
Slurry, is then coated with on plus plate current-collecting body 1 aluminium foil, obtains positive plate after drying.
(2) negative pole lithium sheet, barrier film and positive plate are sticked together insert in CR2032 type button cell shell, at battery case
Interior injection electrolyte, the electrolyte of injection be 1mol/L LiTFSI DOL-DME solution (volume ratio of DOL and DME is 1:
1), seal, obtain CR2032 type button lithium-sulfur cell.
Comparative example 2
(1) sulfur active material, acetylene black, PVDF binding agent are joined in NMP according to the ratio of weight ratio 90:5:5 it is mixed into
Slurry, is then coated with on plus plate current-collecting body 1 aluminium foil, obtains containing the first sulfur carbon coat 2 positive plate after drying.
(2) sulfur active material, Graphene, PVDF binding agent are joined in NMP according to the ratio of weight ratio 10:80:10
It is mixed into slurry, is then coated with on the first sulfur carbon coat 2 positive plate, after drying, obtains positive plate.
(3) negative pole lithium sheet, barrier film and positive plate are sticked together insert in CR2032 type button cell shell, at battery case
Interior injection electrolyte, the electrolyte of injection be 1mol/L LiTFSI DOL-DME solution (volume ratio of DOL and DME is 1:
1), seal, obtain CR2032 type button lithium-sulfur cell.
Effect is as shown in table 1:
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example 1 | Comparative example 2 | |
| Specific discharge capacity (mAh/g) after circulation first | 574 | 569 | 583 | 572 | 593 | 612 | 556 |
| Specific discharge capacity (mAh/g) after 100 circulations | 470 | 472 | 496 | 457 | 492 | 190 | 406 |
| Capability retention after 100 circulations | 82% | 83% | 85% | 80% | 83% | 31% | 73% |
As shown in Table 1, lithium-sulfur cell capacity prepared by the present invention can keep more than 83% after 100 discharge and recharges, relative to just
The most unprotected comparative example 1 and the comparative example 2 of only part protection, capacity retention rate is greatly improved.
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert
Being embodied as of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
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 present invention's
Protection domain.
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 (9)
1. a sulfur positive plate, it is characterised in that include collector and be positioned at the compound painting of the first sulfur carbon being sequentially distributed thereon
Coating, for stopping the second sulfur carbon composite coated layer of sulfur loss in the first sulfur carbon composite coated layer and for stopping the first sulfur carbon
The 3rd composite coated layer that in composite coated layer, sulfur runs off.
2. sulfur positive plate as claimed in claim 1, it is characterised in that the sulfur carbon mass ratio in described second sulfur carbon coat is little
Sulfur carbon mass ratio in the first sulfur carbon composite coated layer.
3. sulfur positive plate as claimed in claim 1, it is characterised in that described second sulfur carbon coat includes Graphene, bonding
Agent and sulfur active material.
4. sulfur positive plate as claimed in claim 1, it is characterised in that during the Graphene in described second sulfur carbon coat has
Pore structure, its aperture is at 5-50nm.
5. sulfur positive plate as claimed in claim 1, it is characterised in that described 3rd composite coated layer includes lithium titanate, graphite
Alkene and binding agent.
6. sulfur positive plate as claimed in claim 1, it is characterised in that the first sulfur carbon coat: the second sulfur carbon coat: the 3rd
The thickness of composite coated layer is than for 100:2-5:5-10.
7. the preparation method preparing lithium sulphur battery electrode sheet as claimed in claim 1, it is characterised in that include following several
Individual step:
Step (1): sulfur active material, conductive agent, binding agent are joined according to the ratio of weight ratio 80-90:5-10:5-10
NMP is mixed into slurry, is then coated with on plus plate current-collecting body aluminium foil, obtain after drying containing the first sulfur carbon coat positive pole
Sheet；
Step (2): sulfur active material, Graphene, binding agent are joined according to the ratio of weight ratio 10-40:40-80:5-10
NMP is mixed into slurry, is then coated with on the first sulfur carbon coat positive plate, obtains after drying containing the second sulfur carbon coat
Positive plate；
Step (3): lithium titanate material, Graphene, binding agent are joined according to the ratio of weight ratio 80-90:5-10:5-10
NMP is mixed into slurry, is then coated with on the second sulfur carbon coat positive plate, after drying, obtains positive plate；
Step (4): by obtained by negative pole lithium sheet, barrier film and step (3) positive plate stick together and insert CR2032 type button
In battery case, in battery case, inject electrolyte, seal, obtain CR2032 type button lithium-sulfur cell.
8. method as claimed in claim 7, it is characterised in that the electrolyte injected in described step (4) is 1mol/L
The DOL-DME solution of LiTFSI.
9. a lithium-sulfur cell, it is characterised in that include lithium anode, barrier film, and sulfur positive pole as claimed in claim 1
Sheet.
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| CN108580143A (en) * | 2018-05-22 | 2018-09-28 | 中国第汽车股份有限公司 | A kind of all-solid lithium-ion battery pole plate gradient spraying equipment and spraying method |
| CN110875496A (en) * | 2018-08-30 | 2020-03-10 | 中南大学 | Metal lithium battery and electrolyte thereof |
| WO2020096253A1 (en) * | 2018-11-08 | 2020-05-14 | 주식회사 엘지화학 | Positive electrode active material for lithium rechargeable battery, manufacturing method therefor and lithium rechargeable battery comprising same |
| CN112514112A (en) * | 2018-11-08 | 2021-03-16 | 株式会社Lg化学 | Positive electrode active material for lithium secondary battery, method for producing same, and lithium secondary battery comprising same |
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| CN112514112A (en) * | 2018-11-08 | 2021-03-16 | 株式会社Lg化学 | Positive electrode active material for lithium secondary battery, method for producing same, and lithium secondary battery comprising same |
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