CN106410098A - Composite lithium-sulfur battery diaphragm - Google Patents
Composite lithium-sulfur battery diaphragm Download PDFInfo
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- CN106410098A CN106410098A CN201610890014.4A CN201610890014A CN106410098A CN 106410098 A CN106410098 A CN 106410098A CN 201610890014 A CN201610890014 A CN 201610890014A CN 106410098 A CN106410098 A CN 106410098A
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- film
- aramid fiber
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- polyurethane
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
-
- 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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- 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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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a composite lithium-sulfur battery diaphragm and belongs to the technical field of lithium-sulfur battery diaphragms. The composite lithium-sulfur battery diaphragm is formed by compounding a layer of aramid fiber film with the thickness of 10-15 microns, a layer of polyurethane film with the thickness of 3-5 microns and a layer of graphene-doped polyvinylidene fluoride film with the thickness of 8-10 microns. A specific preparation method of the composite diaphragm comprises the following steps of (1) adopting an electrospinning technology to prepare the aramid fiber film; (2) utilizing an electrospinning method to prepare polyurethane and preparing a polyurethane/aramid fiber composite film through on-line compounding; and (3) adopting the electrospinning technology to prepare the graphene-doped polyvinylidene fluoride film, and preparing the composite lithium-sulfur battery diaphragm through on-line compounding of the polyvinylidene fluoride film and the polyurethane/aramid fiber composite film. The composite lithium-sulfur battery diaphragm prepared by applying the method plays an important role in the lithium-sulfur battery.
Description
Technical field
The present invention relates to a kind of compound lithium-sulfur cell barrier film, belong to the technical field of lithium-sulfur cell barrier film.
Background technology
With the raising of scientific and technical continuous development and living standards of the people, people propose to the development of serondary lithium battery
Higher demand, especially in terms of high-performance electric motor-car, is badly in need of having high energy storage and an energy output system.Lithium-sulfur cell due to
Have high theoretical specific capacity (1675mAh g-1) and energy density (2600Wh kg-1), obtain Chinese scholars and extensively close
Note.Barrier film is the important component part of lithium-sulfur cell, and it affects chemical property and the security performance of whole battery.Currently, exist
On market, main battery diaphragm includes：Polypropylene, polyethylene and their complex form.But, when these barrier films use
During in the battery being assembled, but the shortcoming of these films is also very notable, such as under high temperature or high current density, charge-discharge performance
Poor, lead to there is larger potential safety hazard, and its lyophily is poor, ionic conductivity is low, especially these barrier films can not be to many
Sulphur compound is effectively suppressed, and therefore develops high performance barrier film and becomes and improves one important side of lithium-sulfur cell performance
Face.
For the problems referred to above, many scholars propose solution.For example, people are by CNT, orderly mesoporous
Carbon nano-particles, Nano carbon balls and Graphene are doped in sulfur positive pole, and these methods can give electrode, and smoothly electronics turns
Mobile Communication road, simultaneously in the starting stage, can suppress the shuttle effect of polysulfide to a certain extent.But because these materials are big
Part is open architecture, and after long-time circulation, polysulfide can not be attracted in positive pole battery effectively.Closely
Come, interlayer is also applied between lithium-sulphur cell positive electrode and barrier film, it can absorb as upper strata collector and polysulfide
Agent, so can suppress the shuttle effect of polysulfide effectively.But interlayer can not and anode and barrier film between closely
In conjunction with peeling off phenomenon easily and between them, therefore it cannot be guaranteed that it is just remaining performance during circulating battery
Normal function, which reduces the seizure effect to polysulfide.Certainly some are in the method for battery diaphragm face coat
Have the shortcomings that the same with cell interlayer introduction, therefore, there is still a need for developing a kind of new barrier film to improve lithium-sulfur cell
Performance.
Content of the invention
The problem existing for above-mentioned background technology, it is an object of the invention to provide compound lithium-sulfur cell barrier film, should
Plant the compatibility that invention can improve barrier film and positive/negative plate.The film being close to anode is the Kynoar mixed with Graphene
Film, can be easy to the transfer of electronics and ion, so greatly reduces the transfger impedance of electric charge as battery upper strata collector, and
And this film can form physical barrier to stop the shuttle effect of polysulfide in lithium-sulfur cell, and the base material being used is poly-
Vinylidene fluoride film, it is easily and electrolyte forms gelation, pick up and the safety of battery diaphragm is greatly improved, is used
Aramid fiber film can provide excellent mechanical property for composite diaphragm.
The present invention provides a kind of compound lithium-sulfur cell barrier film, and described compound lithium-sulfur cell barrier film by a layer thickness is
10～15 μm of aramid fiber film, a layer thickness be 3～5 μm of polyurethane film and a layer thickness be 8～10 μm poly- mixed with Graphene
Vinylidene fluoride film is composited.
Using high-temperature resistant aramid fiber polymeric film as battery barrier film, the heat stability of this battery and safety have obtained pole
Big raising；Spray on the surface of aramid fiber film using polyurethane film, polyurethane film can increase flexibility and the raising of battery diaphragm
The strength of barrier film；Sprayed in the surface of polyurethane/aramid fiber composite membrane, the graphite in polyvinylidene fluoride film using polyvinylidene fluoride film
Alkene can increase the activity of positive electrode, and Kynoar can form gelation effect to increase the reactivity of positive pole and to add
The strong inhibitory action to polysulfide.
The preparation method of described compound lithium-sulfur cell barrier film is it is characterised in that comprise the steps：
(1) aramid fiber film is prepared using electrostatic spinning technique；
(2) prepare polyurethane using electrospinning process, be combined online and prepare polyurethane/aramid fiber composite membrane；
(3) adopt electrostatic spinning technique preparation mixed with Graphene polyvinylidene fluoride film, and by this polyvinylidene fluoride film with
Polyurethane/aramid fiber composite membrane is combined online prepares compound lithium-sulfur cell barrier film.
A kind of compound lithium-sulfur cell barrier film is due to using above technical scheme, the lithium-sulfur cell with this barrier film of invention
Have the characteristics that：
(1) due to using high-temperature resistant aramid fiber polymeric film as battery barrier film, the heat stability of battery and safety obtain
Arrive great raising；
(2) because polyurethane film sprays on the surface of aramid fiber film, it can increase the flexibility of battery diaphragm and improve barrier film
Strength；
(3) because polyvinylidene fluoride film sprays on the surface of polyurethane/aramid fiber composite membrane, Graphene can increase positive pole material
The activity of material, Kynoar can form gelation effect to increase the reactivity of positive pole and to strengthen the suppression to polysulfide
Make and use；
(4) this kind of technology being combined online can make to be formed between trilamellar membrane and preferably combine, and prevent from peeling off between barrier film
With come off, and greatly reduce the internal resistance of battery diaphragm.
Aforementioned four feature make prepared to lithium-sulfur cell there is more excellent chemical property.
The invention provides a kind of compound lithium-sulfur cell barrier film, the lithium-sulfur cell of the composite diaphragm of its preparation can be direct
Hybrid electric vehicle uses, and this method is by for preparation in terms of lithium-sulfur cell for the membrane for polymer gelation and utilization
A kind of new way is provided.
Brief description
Fig. 1 be aramid fiber film/mixed with Graphene Kynoar membrane composite lithium-sulfur cell barrier film preparation flow figure.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment 1
(1) the aramid fiber emulsion being 10wt.% by 10g concentration is added in the dimethyl acetylamide of 7.2g and is mixed with aramid fiber
Spinning solution, prepares aramid fiber film using electrostatic spinning technique, and the technical parameter preparing this aramid fiber film is：Electrostatic spinning voltage
25Kv, a diameter of 0.3mm with the close-connected pin of syringe, the solution quantity delivered of syringe needle remains 0.1ml h-1, syringe
Most advanced and sophisticated spinning distance and catcher between is 15cm；
(2) with DMF, polyaminoester emulsion and a small amount of polyvinylidene fluoride emulsion as raw material, aramid fiber film
For receiver board, prepare polyurethane/aramid fiber composite membrane using known electrospinning process, described DMF,
The quality of polyaminoester emulsion and polyvinylidene fluoride emulsion is respectively 10g, 2g and 1g, and spinning voltage 35Kv is tight with syringe
The a diameter of 0.3mm of pin connecting, the solution quantity delivered of syringe needle remains 0.1mlh-1, spinning between syringe tip and catcher
Flight lead is from for 15cm；
(3) the Kynoar powder of 4.8g and 32ml dimethylformamide are mixed, then the Graphene of 1.75g is added
To in mixed liquor, after uniform stirring, prepare the Kynoar spinning solution mixed with Graphene, with the polyurethane in step (2)/
Aramid fiber composite membrane is receiver board, prepares the polyvinylidene fluoride film mixed with Graphene using electrostatic spinning technique, and this is gathered inclined fluorine
Vinyl film and aramid fiber film are combined online prepares compound lithium-sulfur cell barrier film.Described electrostatic method prepares the ginseng of polyvinylidene fluoride film
Number：Spinning voltage 30Kv, a diameter of 0.3mm with the close-connected pin of syringe, the solution quantity delivered of syringe needle remains 0.1ml
h-1, the spinning distance between syringe tip and catcher is 15cm.
Whole aramid fiber film/polyurethane/mixed with the preparation of polyvinylidene fluoride film composite membrane of Graphene and lithium-sulfur cell group
Dress schematic flow sheet is as shown in Figure 1.Using the composite membrane in above-mentioned steps (3) as lithium-sulfur cell barrier film, it is assembled into battery, and surveys
Try chemical property under the multiplying power of 0.5C for the battery, result is：Initial discharge specific capacity is 1168mAh g-1, 200 circulations
Its specific discharge capacity is 67% afterwards, and it is as shown in table 1.
Embodiment 2
(1) the aramid fiber emulsion being 20wt.% by 10g concentration is added in the dimethyl acetylamide of 7.2g and is mixed with aramid fiber
Spinning solution, prepares aramid fiber film using electrostatic spinning technique, and the technical parameter preparing this aramid fiber film is：Electrostatic spinning voltage
35Kv, a diameter of 0.6mm with the close-connected pin of syringe, the solution quantity delivered of syringe needle remains 0.3ml h-1, syringe
Most advanced and sophisticated spinning distance and catcher between is 25cm；
(2) with DMF, polyaminoester emulsion and a small amount of polyvinylidene fluoride emulsion as raw material, aramid fiber film
For receiver board, prepare polyurethane/aramid fiber composite membrane using known electrospinning process, described DMF,
The quality of polyaminoester emulsion and polyvinylidene fluoride emulsion is respectively 10g, 2g and 1g, and spinning voltage 45Kv is tight with syringe
The a diameter of 0.6mm of pin connecting, the solution quantity delivered of syringe needle remains 0.3ml h-1, spinning between syringe tip and catcher
Flight lead is from for 25cm；
(3) the Kynoar powder of 4.8g and 32ml dimethylformamide are mixed, then the Graphene of 2.81g is added
To in mixed liquor, after uniform stirring, prepare the Kynoar spinning solution mixed with Graphene, with the polyurethane in step (2)/
Aramid fiber composite membrane is receiver board, prepares the polyvinylidene fluoride film mixed with Graphene using electrostatic spinning technique, and this is gathered inclined fluorine
Vinyl film and aramid fiber film are combined online prepares compound lithium-sulfur cell barrier film.Described electrostatic method prepares the ginseng of polyvinylidene fluoride film
Number：Spinning voltage 40Kv, a diameter of 0.3mm with the close-connected pin of syringe, the solution quantity delivered of syringe needle remains 0.1ml
h-1, the spinning distance between syringe tip and catcher is 15cm.
Whole aramid fiber film/polyurethane/mixed with the preparation of polyvinylidene fluoride film composite membrane of Graphene and lithium-sulfur cell group
Dress schematic flow sheet is as shown in Figure 1.Using the composite membrane in above-mentioned steps (3) as lithium-sulfur cell barrier film, it is assembled into battery, and surveys
Try chemical property under the multiplying power of 0.5C for the battery, result is：Initial discharge specific capacity is 1271mAh g-1, 200 circulations
Its specific discharge capacity is 72% afterwards, and it is as shown in table 1.
Embodiment 3
(1) 10g aramid fiber emulsion is added in the dimethyl acetylamide of 7.2g and is mixed with aramid fiber spinning solution, using quiet
Electrospinning prepares aramid fiber film, and the technical parameter preparing this aramid fiber film is：Electrostatic spinning voltage 30Kv, is closely connected with syringe
A diameter of 0.5mm of the pin connecing, the solution quantity delivered of syringe needle remains 0.2ml h-1, spinning between syringe tip and catcher
Flight lead is from for 20cm；
(2) with DMF, polyaminoester emulsion and a small amount of polyvinylidene fluoride emulsion as raw material, aramid fiber film
For receiver board, prepare polyurethane/aramid fiber composite membrane using known electrospinning process, described DMF,
The quality of polyaminoester emulsion and polyvinylidene fluoride emulsion is respectively 10g, 2g and 1g, and spinning voltage 45Kv is tight with syringe
The a diameter of 0.6mm of pin connecting, the solution quantity delivered of syringe needle remains 0.3ml h-1, spinning between syringe tip and catcher
Flight lead is from for 25cm；
(3) the Kynoar powder of 4.8g and 32ml dimethylformamide are mixed, then the Graphene of 3.51g is added
To in mixed liquor, after uniform stirring, prepare the Kynoar spinning solution mixed with Graphene, with the polyurethane in step (2)/
Aramid fiber composite membrane is receiver board, prepares the polyvinylidene fluoride film mixed with Graphene using electrostatic spinning technique, and this is gathered inclined fluorine
Vinyl film and aramid fiber film are combined online prepares compound lithium-sulfur cell barrier film.Described electrostatic method prepares the ginseng of polyvinylidene fluoride film
Number：Spinning voltage 40Kv, a diameter of 0.3mm with the close-connected pin of syringe, the solution quantity delivered of syringe needle remains 0.1ml
h-1, the spinning distance between syringe tip and catcher is 15cm.
Whole aramid fiber film/polyurethane/mixed with the preparation of polyvinylidene fluoride film composite membrane of Graphene and lithium-sulfur cell group
Dress schematic flow sheet is as shown in Figure 1.Using the composite membrane in above-mentioned steps (3) as lithium-sulfur cell barrier film, it is assembled into battery, and surveys
Try chemical property under the multiplying power of 0.5C for the battery, result is：Initial discharge specific capacity is 1386mAh g-1, 200 circulations
Its specific discharge capacity is 82% afterwards, and it is as shown in table 1.
Embodiment 4
(1) 10g aramid fiber emulsion is added in the dimethyl acetylamide of 7.2g and is mixed with aramid fiber spinning solution, using quiet
Electrospinning prepares aramid fiber film, and the technical parameter preparing this aramid fiber film is：Electrostatic spinning voltage 30Kv, is closely connected with syringe
A diameter of 0.5mm of the pin connecing, the solution quantity delivered of syringe needle remains 0.2ml h-1, spinning between syringe tip and catcher
Flight lead is from for 20cm；
(2) with DMF, polyaminoester emulsion and a small amount of polyvinylidene fluoride emulsion as raw material, aramid fiber film
For receiver board, prepare polyurethane/aramid fiber composite membrane using known electrospinning process, described DMF,
The quality of polyaminoester emulsion and polyvinylidene fluoride emulsion is respectively 10g, 2g and 1g, and spinning voltage 45Kv is tight with syringe
The a diameter of 0.6mm of pin connecting, the solution quantity delivered of syringe needle remains 0.3ml h-1, spinning between syringe tip and catcher
Flight lead is from for 25cm；
(3) the Kynoar powder of 4.8g and 32ml dimethylformamide are mixed, then the Graphene of 5.27g is added
To in mixed liquor, after uniform stirring, prepare the Kynoar spinning solution mixed with Graphene, with the polyurethane in step (2)/
Aramid fiber composite membrane is receiver board, prepares the polyvinylidene fluoride film mixed with Graphene using electrostatic spinning technique, and this is gathered inclined fluorine
Vinyl film and aramid fiber film are combined online prepares compound lithium-sulfur cell barrier film.Described electrostatic method prepares the ginseng of polyvinylidene fluoride film
Number：Spinning voltage 40Kv, a diameter of 0.3mm with the close-connected pin of syringe, the solution quantity delivered of syringe needle remains 0.1ml
h-1, the spinning distance between syringe tip and catcher is 15cm.
Whole aramid fiber film/polyurethane/mixed with the preparation of polyvinylidene fluoride film composite membrane of Graphene and lithium-sulfur cell group
Dress schematic flow sheet is as shown in Figure 1.Using the composite membrane in above-mentioned steps (3) as lithium-sulfur cell barrier film, it is assembled into battery, and surveys
Try chemical property under the multiplying power of 0.5C for the battery, result is：Initial discharge specific capacity is 1298mAh g-1, 200 circulations
Its specific discharge capacity is 76% afterwards, and it is as shown in table 1.
Based on aforementioned four case study on implementation, according to the fineness of spinning fibre, the uniformity, degree of crystallinity, the porosity of film and suction
(within the specific limits, fibre fineness is thinner, the uniformity is more uniform, degree of crystallinity is less and the porosity of film and pick up for liquid rate
More big prepared film properties are more beneficial for battery performance) etc. index understand：When preparation is mixed with the polyvinylidene fluoride film of Graphene
When, during the Graphene of selection doping 10%, barrier film has the performance being preferably beneficial to battery, and passes through the various embodiments described above electrochemistry
Test also illustrates in embodiment 3 with respect to other three more favourable battery performances.
The foregoing is only the preferred embodiments of the present invention, not thereby limit the scope of the claims using the present invention.This
In bright embodiment assembling battery under the multiplying power of 0.5C, battery initial discharge specific capacity and circulation 200 times after remaining electric discharge
Specific capacity percentage ratio is as shown in table 1：
In table 1 aforementioned four embodiment, the battery of assembling is under the multiplying power of 0.5C, battery initial discharge specific capacity and circulation
Remaining specific discharge capacity percentage ratio after 200 times
Claims (2)
1. a kind of compound lithium-sulfur cell barrier film, the virtue that described compound lithium-sulfur cell barrier film is 10～15 μm by a layer thickness
Synthetic fibre film, a layer thickness is 3～5 μm of polyurethane film and a layer thickness is that 8～10 μm of polyvinylidene fluoride films mixed with Graphene are multiple
Conjunction forms.
2. as claimed in claim 1 compound lithium-sulfur cell barrier film preparation method it is characterised in that：Described the gathering partially of preparation
In fluoride film Static Spinning film, the quality of Kynoar powder and the volume ratio of dimethylformamide meet 0.15g/ml, institute
The Graphene using is the quality of this two kinds of mixed liquors is 5%～15%.
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| CN201610890014.4A CN106410098A (en) | 2016-10-11 | 2016-10-11 | Composite lithium-sulfur battery diaphragm |
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| CN201610890014.4A CN106410098A (en) | 2016-10-11 | 2016-10-11 | Composite lithium-sulfur battery diaphragm |
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Cited By (6)
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| CN107579191A (en) * | 2017-08-18 | 2018-01-12 | 哈尔滨工业大学 | A kind of preparation method and applications of lithium-sulfur cell porous composite film |
| CN108505213A (en) * | 2018-05-14 | 2018-09-07 | 广东石油化工学院 | A kind of preparation method of amino graphene/polyunsymfluorethylepiezoelectric piezoelectric nanometer electrospinning film |
| CN109755446A (en) * | 2018-12-10 | 2019-05-14 | 沈阳化工大学 | A kind of lithium-sulfur cell diaphragm and preparation method thereof |
| CN109786619A (en) * | 2017-11-13 | 2019-05-21 | 北京碳阳科技有限公司 | A kind of battery diaphragm and preparation method thereof |
| CN110010823A (en) * | 2019-03-14 | 2019-07-12 | 扬州大学 | Lithium-sulfur cell diaphragm material, preparation method and applications |
| CN110556493A (en) * | 2019-08-13 | 2019-12-10 | 中国科学院化学研究所 | Functional composite diaphragm of lithium/sodium secondary battery and preparation method thereof |
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| CN107579191A (en) * | 2017-08-18 | 2018-01-12 | 哈尔滨工业大学 | A kind of preparation method and applications of lithium-sulfur cell porous composite film |
| CN107579191B (en) * | 2017-08-18 | 2020-08-07 | 哈尔滨工业大学 | Preparation method and application of porous composite membrane of lithium-sulfur battery |
| CN109786619A (en) * | 2017-11-13 | 2019-05-21 | 北京碳阳科技有限公司 | A kind of battery diaphragm and preparation method thereof |
| CN108505213A (en) * | 2018-05-14 | 2018-09-07 | 广东石油化工学院 | A kind of preparation method of amino graphene/polyunsymfluorethylepiezoelectric piezoelectric nanometer electrospinning film |
| CN108505213B (en) * | 2018-05-14 | 2019-08-13 | 广东石油化工学院 | A kind of preparation method of amino graphene/polyunsymfluorethylepiezoelectric piezoelectric nanometer electrospinning film |
| CN109755446A (en) * | 2018-12-10 | 2019-05-14 | 沈阳化工大学 | A kind of lithium-sulfur cell diaphragm and preparation method thereof |
| CN109755446B (en) * | 2018-12-10 | 2021-11-23 | 沈阳化工大学 | Lithium-sulfur battery diaphragm and preparation method thereof |
| CN110010823A (en) * | 2019-03-14 | 2019-07-12 | 扬州大学 | Lithium-sulfur cell diaphragm material, preparation method and applications |
| CN110556493A (en) * | 2019-08-13 | 2019-12-10 | 中国科学院化学研究所 | Functional composite diaphragm of lithium/sodium secondary battery and preparation method thereof |
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