CN105870493A - Lithium-sulfur battery, lithium-sulfur battery intermediate and preparation method thereof - Google Patents
Lithium-sulfur battery, lithium-sulfur battery intermediate and preparation method thereof Download PDFInfo
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- CN105870493A CN105870493A CN201610311564.6A CN201610311564A CN105870493A CN 105870493 A CN105870493 A CN 105870493A CN 201610311564 A CN201610311564 A CN 201610311564A CN 105870493 A CN105870493 A CN 105870493A
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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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention is applicable to the field of lithium-sulfur batteries and provides a preparation method of a lithium-sulfur battery intermediate. The method includes steps: mixing an organic solvent with a non-solvent liquid according to a mass ratio to obtain a mixed liquid, adding a conductive polymer and a nonconductive polymer into the mixed liquid, and stirring at the temperature of 35-60DEG C; standing to remove bubbles to obtain a film casting liquid; coating a film forming substrate with the film casting liquid, and drying under a vacuum condition to obtain the intermediate which is a composite polymer film with micropores 5-25nm in diameter. The invention further provides the lithium-sulfur battery intermediate and a lithium-sulfur battery. After the solid-state lithium-sulfur battery intermediate which is the composite polymer film is positioned between a solid-state electrolyte and an anode material, Sn<2-> of the anode material can be prevented from diffusing out of the surface of the anode material and gathering on the surface of an electrode material, and Li<+> transmission is facilitated. Therefore, capacity and cycle performance of the solid-state lithium-sulfur battery are improved.
Description
Technical field
The invention belongs to lithium-sulfur cell field, particularly relate to a kind of lithium-sulfur cell intermediate and preparation method thereof,
Lithium-sulfur cell.
Background technology
Lithium-sulfur cell is with lithium metal as negative pole, and sulphurous materials is the lithium-sulfur rechargeable battery of positive active material.
The theoretical specific capacity of sulfur is up to 1672mAh/g, voltage 2.2V (vs Li+/ Li), it is to realize high-energy at present
The preferred material that density is current, its actual attainable energy density is 500Wh/kg, solid electrolyte
Lithium-sulfur cell performance is more preferably.Additionally, elemental sulfur low cost, environmentally friendly, meet electric automobile, space
The field such as technology and defence equipment is to electrokinetic cell demand.But lithium-sulfur cell still suffers from two subject matters:
First, positive electrode active material utilization is low, and on the one hand main cause is to be soluble in the middle product of organic electrolyte
Thing polysulfide ion Sn2-The effect of shuttling back and forth of (3≤n≤8), on the other hand discharging product Li2S is after repeatedly circulation
Positive electrode surface, Li can be deposited on2S, owing to having insulating properties, can hinder the electric charge of S positive pole to transmit, and causes having
The loss of effect active substance.Second, multiplying power and the cycle performance of lithium-sulfur cell are poor, and the electrical conductivity of elemental sulfur is low by (5
×10-30S/cm), and positive and negative pole material and electrolyte to contact internal resistance big, be unfavorable for Li+Transmission.
Promote at present positive electrode electric conductivity and mainly use S-C doping techniques, this skill upgrading positive pole
The electrical conductivity of material, but dissolution and the Li of polysulfides cannot be solved2S、Li2S2In electrode material surface
Enrichment phenomenon, eventually result in Li+Transmission be obstructed, in turn result in the decay of discharge capacity of the cell.
Summary of the invention
In order to solve the problems referred to above, the present invention provides a kind of lithium-sulfur cell intermediate and preparation method thereof, lithium sulfur
Battery, it is intended to reduce the dissolution problem of the active substances in cathode materials of lithium-sulfur cell, promotes the appearance of lithium-sulfur cell
Amount and cycle performance.
The present invention is achieved in that the preparation method of a kind of lithium-sulfur cell intermediate, comprises the following steps:
Organic solvent and non solvent liquid are mixed to obtain mixed liquor in mass ratio, by conducting polymer with non-conductive
Polymer adds in described mixed liquor, stirs at a temperature of 35-60 DEG C；
Stand, slough bubble, obtain casting solution；And
Described casting solution is spread upon on film base material, is dried under vacuum, obtain intermediate；
Described intermediate is compound thin polymer film, containing micropore on described thin polymer film, described micro-
The size in hole is 5-25nm.
Present invention also offers a kind of lithium-sulfur cell intermediate, use above-mentioned preparation method to make.
Present invention also offers a kind of lithium-sulfur cell, including above-mentioned lithium-sulfur cell intermediate.
The present invention compared with prior art, has the beneficial effects that: the lithium-sulfur cell intermediate that the present invention provides,
It is one layer of composite polymer films, because it has substantial amounts of micropore and proper pore size, beneficially Li+Transmission；
This intermediate is placed between solid electrolyte and positive electrode, positive electrode S can be stoppedn 2-Diffuse out
Positive electrode surface and avoid its electrode material surface be enriched with；Therefore prepared intermediate improves solid-state
The capacity of lithium-sulfur cell and cycle performance.Further, by adding inorganic receiving in intermediate preparation process
Rice corpuscles, makes to be prepared into composite polymer films and has higher mechanical strength, can just preferably support,
Negative plate.Additionally, the lithium-sulfur cell solid electrolyte of preparation is identical with compound microporous polymer film selection
Polymeric matrix, make many empty polymer film layers better contact with solid electrolyte.
Accompanying drawing explanation
Fig. 1 is the profile of the lithium-sulfur cell that the embodiment of the present invention 1 provides.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and reality
Execute example, the present invention is further elaborated.Only should be appreciated that specific embodiment described herein
Only in order to explain the present invention, it is not intended to limit the present invention.
Liquid electrolyte inflammable, reveal, the safety issue such as blast, exploitation solid electrolyte can solve lithium
The safety issue of ion secondary battery.But solid electrolyte is poor with the direct contact performance of positive and negative pole material,
Internal resistance is high.Modify one layer on positive electrode surface and be conducive to Li+The thin film of transmission, stops Sn 2-Diffusion, can
To reach to increase the purpose of battery capacity.Therefore the present invention adds between S-C positive electrode/solid electrolyte
One layer of Li+Transport layer, and prepare the solid electrolyte of a kind of high conductivity, alleviate the dissolution of polysulfides with
And Li2S、Li2S2In the enrichment of electrode material surface, thus promote capacity and the cyclicity of solid-state lithium-sulfur cell
Energy.
Prepare lithium-sulfur cell intermediate according to technical scheme, comprise the following steps:
It is 90～99:1 to mix to obtain mixed liquor, by conducting polymer by organic solvent and non solvent liquid mass ratio
Add in described mixed liquor with non-conductive polymer, stir at a temperature of 35-60 DEG C；
Stand 20-30min, slough bubble, obtain casting solution；And
Casting solution is spread upon on film base material, be dried under vacuum, obtain intermediate；
Described intermediate is compound thin polymer film, containing a large amount of micropores on described thin polymer film, and institute
The size stating micropore is 5-25nm.
It is used for preparing lithium-sulfur cell by the lithium-sulfur cell intermediate of gained.
Specifically, organic solvent is the one in acetone, oxolane, described non solvent liquid be ethanol,
One in water, n-butyl alcohol.Conducting polymer is PPY (polypyrrole), PTP (polythiophene), PAN
One in (polyaniline), conduction non-conductive polymer is PEO (Pluronic F-127), PAN (poly-third
Alkene nitrile), PMMA (polymethyl methacrylate), P (VDF-HPF) (poly-(vinylidene-hexafluoro third
Alkene)) in one；The boiling point of described non solvent liquid is higher than the boiling point of described organic solvent.Described conduction
Polymer is 1～5:1 with the mass ratio of non-conductive polymer.The temperature being dried under described vacuum condition is preferred
80℃.Use and heat under vacuum condition, make polymer dissolve and form homogeneous phase solution in a solvent.Organic
Solvent boiling point is low, and non solvent liquid boiling point is high, has in high lower boiling two kinds of solvents and adds polymer, stream
Prolonging the evaporation of film forming post-heating, lower boiling solvent evaporation rate is fast, and high boiling non-solvent evaporation rate is slow,
Make thin polymer film and non-solvent occur to be separated and form microporous membrane, prepare the thickness of this thin film
Scope is between 0.1-10 μm, and the most relatively thin how empty thin polymer film is to reduce the internal resistance of lithium-sulfur cell.
Lithium-sulfur cell intermediate prepared by the present invention, is one layer of compound microporous polymer film layer, application
Between the positive electrode and solid electrolyte of lithium-sulfur cell, both can hinder positive electrode Sn 2-Diffusion,
Cavernous structure is conducive to again Li simultaneously+Transmission.In the microporous polymer prepared in the present invention, micropore forms
Li+The passage of transmission, described non-conductive polymer is the organic matrix of passage.Described non-conductive polymerization
Thing degree of crystallinity is the highest, during less than glass transition temperature, easily crystallizes, tends to interfere with Li+Transmission.And it is micro-
Cell polymeric plays the effect of isolation positive and negative pole material in solid state battery, and it is sufficiently strong that this just requires that it has
Mechanical strength support positive/negative plate.The present invention adds one further in described lithium-sulfur cell intermediate
Determine the inorganic nano-particle of quality to increase the mechanical strength of porous compound polymer thin film.
Specifically, being also added with organic/inorganic nano particle in described mixed liquor, described inorganic nano-particle is TiO2、
Al2O3、SiO2、ZrO2, at least one in MgO, CuO；Described inorganic nano-particle is in described mixing
Mass content in liquid is 2～5wt%.Inorganic nano-particle, preparation is added in the preparation process of intermediate
The porous compound polymer thin film mechanical strength that goes out is high, for 5-20MPa, preferably 10-18MPa, it addition, thin
The electrical conductivity of film is 10-3～3mS/cm.
Specifically, preparation lithium-sulfur cell in, solid electrolyte matrix select PEO, PAN, PMMA,
One or two kinds of in P (VDF-HPF), LiN (CF selected by lithium salts3SO2)2、LiTFSi、LiClO4、LiPF6
In at least one, solvent selects NMP or acetonitrile, and plasticizer selects ethylene carbonate, Allyl carbonate
Or the one in dibutylphosphoric acid ester.As preferably, this lithium-sulfur cell solid electrolyte and compound microporous polymer
The polymeric matrix that the selection of thing thin film is identical, beneficially porous polymer film layer are good with solid electrolyte
Contact.This electrolytic conductivity contacted with composite microporous polymer thin film of this lithium-sulfur cell is more than
10-3S/cm。
In the lithium-sulfur cell of preparation, between positive electrode and solid electrolyte, prepare one layer of polymeric porous
Thin film, this thin film uses polymer add inorganic nanoparticles and prepared by phase transfer of technology, this polymerization
Thing porous membrane plays obstruction S between lithium sulfur battery anode material and solid electrolyten 2-Diffusion.This is multiple
Close the polymer porous membrane partial relaxation by polymer and polymer chain forging motion realizes Li+Transmission, poly-
Functional group that in polymer segments, electronegativity is big and Li+Complexation, under electric field action, along with polymer segments heat is transported
Dynamic, the Li of electrolyte+Dissociate with polymer, then with other segment generation complexation, thus realize lithium ion
Directional migration.Add inorganic nanoparticles and be conducive to the formation of polymer amorphous area and the lifting of mechanical performance,
Reach to promote battery capacity and the purpose of high rate performance.
Below in conjunction with specific embodiment, technical scheme is illustrated.
Embodiment 1
Preparing lithium-sulfur cell intermediate, process is as follows:
(1) organic solvent-acetone and non-solvent ethanol are formed mixed liquor, stir；Then conduction is gathered
Compound polyacrylonitrile (PAN) and non-conductive polymer P (VDF-HPF) join above-mentioned mixing according to 1:1 ratio
In liquid, stir；Wherein, two kinds of polymer mass content in mixed liquor is 5%；
(2) in mixed liquor, 2wt%TiO is added2, it is dispersed therein, constant temperature stirring at 40 DEG C；
(3) bubble is sloughed after standing 20-30min, with the sheet of smooth pieces for one-tenth film base material, on base material
Smear one layer of casting solution；
(4) the one-tenth film base material after casting film is transferred in vacuum drying oven be dried at 80 DEG C 12h, obtains lithium sulfur
Battery intermediate.
The lithium-sulfur cell intermediate of gained is one layer of polymeric thin film, containing a large amount of micropores on thin polymer film,
The size of micropore is 5nm；The thickness of thin polymer film is 0.5 μm；The conductance of described thin polymer film
Rate is 1.2mS/cm；The mechanical strength of thin polymer film is 12MPa.
The microporous polymer film of gained is prepared solid-state lithium-sulfur cell, for battery A.Fig. 1 is battery A's
Profile, 1 is polymer porous membrane, and 2 is anode (aluminium foil), and 3 is S-C positive electrode, 4
Being solid electrolyte, 5 is battery cathode (lithium sheet).It can be seen that prepared microporous polymer
Thing thin layer, between the positive electrode and solid electrolyte of lithium-sulfur cell, plays obstruction positive electrode Sn 2-
Diffusion, be conducive to the most again Li simultaneously+The effect of transmission.
Embodiment 2
(1) conducting polymer PPy and non-conductive polymer PEO is added organic solvent according to 1:1 ratio
In THF and non-solvent water, the content of two kinds of polymer is 7wt%, and at 40 DEG C, constant temperature stirring makes it dissolve；
(2) inorganic nano additive selects 4%wt%MgO to be scattered in above-mentioned suspension, continues stirring
Form homogeneous phase solution；
(3) bubble is sloughed after standing 20-40min, with the sheet of smooth pieces for one-tenth film base material, on base material
Smear certain thickness casting solution；
(4) lithium-sulfur cell intermediate is obtained after proceeding to vacuum drying oven is dried 12h at 80 DEG C.
The lithium-sulfur cell intermediate of gained is one layer of polymeric thin film, containing a large amount of micropores on thin polymer film,
The size of micropore is 24nm；The thickness of thin polymer film is 5 μm；The conductance of described thin polymer film
Rate is 2.5mS/cm；The mechanical strength of thin polymer film is 10MPa.
The microporous polymer film of gained is prepared solid-state lithium-sulfur cell, for battery B.
Embodiment 3
(1) conducting polymer PPy and non-conductive polymer PEO is added organic solvent according to 1:1 ratio
In THF and non-solvent water, the content of two kinds of polymer is 8wt%, and at 40 DEG C, constant temperature stirring makes it dissolve；
(2) inorganic nano additive selects 5%wt%MgO to be scattered in above-mentioned suspension, continues stirring
Form homogeneous phase solution；
(3) bubble is sloughed after standing 20-40min, with the sheet of smooth pieces for one-tenth film base material, on base material
Smear certain thickness casting solution；
(4) lithium-sulfur cell intermediate is obtained after proceeding to vacuum drying oven is dried 12h at 80 DEG C.
The lithium-sulfur cell intermediate of gained is one layer of polymeric thin film, containing a large amount of micropores on thin polymer film,
The size of micropore is 5nm；The thickness of thin polymer film is 5 μm；The electrical conductivity of described thin polymer film
For 0.8mS/cm；The mechanical strength of thin polymer film is 18MPa.
The microporous polymer film of gained is prepared solid-state lithium-sulfur cell, for battery C.
Comparative example 1
Conventional lithium-sulfur cell is designated as battery D.
By battery A, B, C, D carry out volume test, test they capacity after 0.2C circulates 50 weeks
Conservation rate, result such as table 1 below.
Table 1
| Battery type | Battery A | Battery B | Battery C | Battery D |
| Capability retention | 91% | 95% | 88% | 80% |
Test result from embodiment 1, the parameter of the thin polymer film prepared in 2,3 and table 1 understands,
In thin polymer film preparation process: material therefor is different from preparation parameter, to the thin polymer film prepared
Performance can have a certain impact；Add inorganic nano-particle and can improve mechanical performance and the appearance of thin polymer film
Amount conservation rate.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all at this
Any amendment, equivalent and the improvement etc. made within bright spirit and principle, should be included in the present invention
Protection domain within.
Claims (10)
1. the preparation method of a lithium-sulfur cell intermediate, it is characterised in that comprise the following steps:
Organic solvent and non solvent liquid are mixed to obtain mixed liquor in mass ratio, by conducting polymer with non-conductive
Polymer adds in described mixed liquor, stirs at a temperature of 35-60 DEG C；
Stand, slough bubble, obtain casting solution；And
Described casting solution is spread upon on film base material, is dried under vacuum, obtain intermediate；
Described intermediate is compound thin polymer film, containing micropore on described thin polymer film, described micro-
The size in hole is 5-25nm.
2. the preparation method of intermediate as claimed in claim 1, it is characterised in that described organic solvent is
One in acetone, oxolane, described non solvent liquid is the one in ethanol, water, n-butyl alcohol；Have
Machine solvent and non solvent liquid are 90～99:1 in mass ratio.
3. the preparation method of intermediate as claimed in claim 1, it is characterised in that described conducting polymer
For the one in PPY, PTP, PAN, described non-conductive polymer is PEO, PAN, PMMA,
One in P (VDF-HPF)；Described conducting polymer is 1～5:1 with the mass ratio of non-conductive polymer.
4. the preparation method of intermediate as claimed in claim 1, it is characterised in that in described mixed liquor also
Being added with inorganic nano-particle, described inorganic nano-particle is TiO2、Al2O3、SiO2、ZrO2、MgO、
At least one in CuO；Described inorganic nano-particle content in described mixed liquor is 2～5wt%.
5. the preparation method of intermediate as claimed in claim 1, it is characterised in that described non solvent liquid
Boiling point higher than the boiling point of described organic solvent.
6. a lithium-sulfur cell intermediate, it is characterised in that use described in Claims 1 to 5 any one
Preparation method make.
7. intermediate as claimed in claim 6, it is characterised in that the thickness of described thin polymer film is
0.1-10μm；The electrical conductivity of described thin polymer film is 10-3～3mS/cm.
8. intermediate as claimed in claim 6, it is characterised in that the mechanical strength of described thin polymer film
For 5-20MPa.
9. a lithium-sulfur cell, it is characterised in that include the centre described in claim 6～8 any one
Body.
10. lithium-sulfur cell as claimed in claim 9, it is characterised in that described lithium-sulfur cell includes solid-state
Electrolyte, the electrical conductivity of described solid electrolyte is more than 10-3S/cm。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110492169A (en) * | 2019-08-15 | 2019-11-22 | 中山大学 | All solid state lithium-sulfur cell of a kind of welded type integration and preparation method thereof |
| CN111804148A (en) * | 2020-06-29 | 2020-10-23 | 浙江美易膜科技有限公司 | High-porosity hydrophilic microporous membrane, preparation method and application thereof |
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| CN103531840A (en) * | 2013-11-01 | 2014-01-22 | 中国科学院上海硅酸盐研究所 | Double-electrolyte system lithium sulphur battery and preparing method thereof |
| CN103665678A (en) * | 2012-08-28 | 2014-03-26 | 苏州宝时得电动工具有限公司 | Polymer film and preparation method thereof, electrolyte provided with polymer film and battery |
| CN105489815A (en) * | 2016-01-15 | 2016-04-13 | 中南大学 | Interlayer used for all-solid-state lithium sulfur battery and all-solid-state lithium sulfur battery |
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2016
- 2016-05-12 CN CN201610311564.6A patent/CN105870493A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665678A (en) * | 2012-08-28 | 2014-03-26 | 苏州宝时得电动工具有限公司 | Polymer film and preparation method thereof, electrolyte provided with polymer film and battery |
| CN103531840A (en) * | 2013-11-01 | 2014-01-22 | 中国科学院上海硅酸盐研究所 | Double-electrolyte system lithium sulphur battery and preparing method thereof |
| CN105489815A (en) * | 2016-01-15 | 2016-04-13 | 中南大学 | Interlayer used for all-solid-state lithium sulfur battery and all-solid-state lithium sulfur battery |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110492169A (en) * | 2019-08-15 | 2019-11-22 | 中山大学 | All solid state lithium-sulfur cell of a kind of welded type integration and preparation method thereof |
| CN110492169B (en) * | 2019-08-15 | 2022-12-23 | 中山大学 | Welding type integrated all-solid-state lithium-sulfur battery and preparation method thereof |
| CN111804148A (en) * | 2020-06-29 | 2020-10-23 | 浙江美易膜科技有限公司 | High-porosity hydrophilic microporous membrane, preparation method and application thereof |
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