CN107994257A - A kind of high-performance solid electrolyte and preparation method thereof - Google Patents
A kind of high-performance solid electrolyte and preparation method thereof Download PDFInfo
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- CN107994257A CN107994257A CN201711447568.8A CN201711447568A CN107994257A CN 107994257 A CN107994257 A CN 107994257A CN 201711447568 A CN201711447568 A CN 201711447568A CN 107994257 A CN107994257 A CN 107994257A
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- electrolyte
- lithium
- solid
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- polycaprolactone
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0082—Organic polymers
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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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- Chemical Kinetics & Catalysis (AREA)
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- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Dispersion Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention provides a kind of high-performance solid electrolyte and preparation method thereof.The high conductivity solid electrolyte, including：Lithium salts and the polymer molecule that lithium ion can be led.Solid polymer electrolyte of the present invention has the advantages that synthetic method is simple, electrical conductivity is high, small with the interface stability of positive/negative electrode material contacts and interface impedance at room temperature.The invention also discloses the method for preparing polymer electrolytes, preparation process is to be dissolved in lithium salts, polymer in solvent according to a certain percentage, then solvent is placed in Teflon mould, it is vacuum dried again after being dried in air dry oven, obtain solid polymer electrolyte material.The solid lithium ion battery assembled using solid polymer of the present invention has good cycle performance.Step is simple and convenient to operate, is highly practical.
Description
Technical field
The invention belongs to field of lithium ion battery, more particularly to a kind of high-performance solid electrolyte and preparation method thereof.
Background technology
As a kind of main electrochemical energy storing device, lithium ion battery has energy density height, charging rate is fast, puts certainly
Electric rate is low, have extended cycle life and memory-less effect etc. a little, in digital camera, laptop, smart mobile phone and bracelet
And it is widely used on the portable electric appts such as Google glass.In addition, lithium ion battery is in hybrid vehicle
Huge potentiality are also shown with fields such as electric automobiles.For example, by lithium ion battery function tesla's electric automobile
It is commercialized through realizing.Conventional lithium ion battery is mainly made of cathode, anode and electrolyte three parts, and wherein electrolyte is as lithium
The passage that ion conducts between positive and negative anodes, plays highly important role.Electrolyte directly affects lithium ion battery
Capacity, temperature in use, security and cycle performance index.Electrolyte system of the solid electrolyte as a kind of high safety, has
Avoid internal short-circuit of battery, prevent electrolyte leakage, without unique advantages such as inflammable and explosive components, before showing wide application
Scape, makes it receive the extensive concern of a large amount of domestic and international researchers.Moreover, the decomposition voltage of solid electrolyte compares liquid electrolytic
The high nearly 1V of matter, therefore the energy density of battery can be improved.Current CN106450443A discloses a kind of PEO based polyalcohols electricity
The method for solving matter, PEO, nano-oxide, lithium salts are dispersed in acetonitrile, mixed liquor is poured in the mould of polytetrafluoroethylene (PTFE),
Spontaneously dry, finally prepared the polymer electrolyte film of micron order thickness, improved the electrical conductivity of polymer dielectric；
CN106410270A discloses lithium single-ion conductor solid polymer electrolyte that a kind of carbonic ester is main chain and preparation method thereof,
M-Li therein+For COOLi or SO3Li et al., simple and practicable, raw material is cheap and easily-available, ring with synthesizing for polymer single ion electrolyte
The advantages that border is friendly.
Most of lithium ion conduction is all to use the solid polymer electrolyte based on polyethylene oxide (PEO), it
There is the shortcomings that easy crystallization, cause conductivity at room temperature relatively low, so unavailable at room temperature.
The content of the invention
In order to overcome above-mentioned deficiency, the present invention provides a kind of high-performance solid electrolyte and preparation method thereof.What is used answers
Mould assembly solid polymer electrolyte, there is higher ionic conductivity at room temperature, and can be with commercialization LiFePO4 just
There is good compatibility in pole, can form stable SEI films.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of solid polymer electrolyte, the electrolyte with the polymer and lithium salts of leading lithium ion ability by forming；
Wherein, it is described to have that to lead the polymer of lithium ion ability be polytrimethylene carbonate PTMC and polycaprolactone (PCL)
Mixture.
Preferably, the polytrimethylene carbonate and the mass ratio of polycaprolactone are 0.05~5：1.
Preferably, the mass fraction of lithium salts is 10%~50% in the electrolyte, has the polymerization for leading lithium ion ability
The mass fraction of thing in the electrolyte is 50%~90%.
Preferably, the molecular weight of the polytrimethylene carbonate is 0.1 ten thousand~200,000.
Preferably, the molecular weight of the polycaprolactone is 20,000~120,000.
Preferably, the lithium salts is LiTFSI, LiPF6、LiClO4、LiAsF6、LiBF4、LiCH3SO3、LiCF3SO3、
LiBO、LiN(CF3SO2)2At least one of.
Present invention also offers a kind of preparation method of solid polymer electrolyte, including：
At ambient temperature, lithium salts, polytrimethylene carbonate PTMC and polycaprolactone (PCL) are dissolved in acetonitrile or acetone
In, it is uniformly mixed, through drying twice, up to solid electrolyte film.
Preferably, it is described dry twice to concretely comprise the following steps：With 70 DEG C of dry 12~24h in air dry oven, then
It is transferred in vacuum drying chamber with 60 DEG C of dry 8~16h.
Present invention also offers a kind of all-solid lithium-ion battery, by cathode, anode and between cathode and anode
Electrolyte composition, electrolyte uses any above-mentioned solid polymer electrolyte, and cathode includes：Positive electrode active materials, afflux
Body, conductive agent and binding agent；Anode includes negative active core-shell material, collector, conductive agent and binding agent.
Preferably, the positive electrode active materials include：Cobalt acid lithium, LiMn2O4, LiFePO4, lithium-nickel-cobalt-oxygen, lithium nickel cobalt manganese
Oxygen, lithium ferric manganese phosphate.
Solid polymer electrolyte of the present invention has that synthetic method is simple, electrical conductivity is high at room temperature and positive/negative
The advantages that interface stability and small interface impedance of electrode material contacts.The invention also discloses the preparation of the polymer dielectric
Then solvent is placed in polytetrafluoroethylene (PTFE) mould by method, preparation process for lithium salts, polymer are dissolved in solvent according to a certain percentage
It is vacuum dried again after being dried in air dry oven in tool, obtain solid polymer electrolyte material.Using of the present invention
Solid polymer assembling solid lithium ion battery there is good cycle performance.
Beneficial effects of the present invention
(1) the two kinds of polymer raw material (polytrimethylene carbonate and polycaprolactone) used in the present invention, which has, biological to drop
The characteristics of solution, environmentally protective and hypotoxicity.
(2) preparation method of compound polymer electrolyte provided by the present invention is simple with preparation process, and cost is low
The advantages that.
(3) mechanical performance is paid no attention to when polytrimethylene carbonate provided by the present invention independently forms a film at ambient temperature
Think；The polycaprolactone of offer is semi-crystalline polymer at room temperature, and ionic conductivity is undesirable.The present invention is by two kinds of polymer
The compound polymer electrolyte obtained after mixing has electrical conductivity height, good mechanical performance and positive/negative electrode material at room temperature
The advantages that expecting the interface stability of contact.
(4) all-solid lithium-ion battery provided by the present invention has stable SEI films, room temperature can use, cyclicity is got well etc.
Advantage.
(5) preparation method of the present invention is simple, electrical efficiency is high, highly practical, easy to spread.
Brief description of the drawings
The accompanying drawings which form a part of this application are used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are used to explain the application, do not form the improper restriction to the application.
Fig. 1 is the lithium ion battery of the solid electrolyte assembling provided in an embodiment of the present invention using embodiment 1 in room temperature
20 DEG C of loop test.
Fig. 2 is the lithium ion battery of the solid electrolyte assembling provided in an embodiment of the present invention using embodiment 1 in room temperature
20 DEG C of charging and discharging curve.
Embodiment
It is noted that described further below is all illustrative, it is intended to provides further instruction to the application.It is unless another
Indicate, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
As background technology is introduced, in the prior art, there are technique is cumbersome, processing for the preparation of porous silicon composite material
Efficiency is low, the problem such as lower than energy, and to solve the above-mentioned problems, the present invention provides a kind of metallic cover porous silicon composite electrode
Material and preparation method thereof, with reference to specific embodiment, the present invention is described further.
A kind of solid polymer electrolyte, forms and is：With polymer, the lithium salts for leading lithium ion ability；It is characterized in that：
The mass fraction of lithium salts is 10%~50% in the solid polymer electrolyte, has the polymer for leading lithium ion ability in electricity
It is 50%~90% to solve the mass fraction in matter.
The lithium salts is LiTFSI, LiPF6、LiClO4、LiAsF6、LiBF4、LiCH3SO3、LiCF3SO3、LiBO、LiN
(CF3SO2)2At least one therein.
Described have that to lead the polymer of lithium ion ability be polytrimethylene carbonate (PTMC) and polycaprolactone (PCL)
Mixture.
The molecular weight of the polytrimethylene carbonate is 0.1 ten thousand~200,000.
The molecular weight of the polycaprolactone is 20,000~120,000.
It is described have the polytrimethylene carbonate for leading lithium ion ability and the mass ratio of polycaprolactone for 0.05~
5：1.
The preparation method is as follows：First, lithium salts and two kinds of polymer are dissolved in acetonitrile or third at ambient temperature
In ketone, stirring is transferred in Teflon mould to after forming uniform solution, then dry with 70 DEG C in air dry oven
Dry 12~24h, is then transferred in vacuum drying chamber with 60 DEG C of dry 8~16h, obtains solid electrolyte film.
A kind of all-solid lithium-ion battery, is made of cathode, anode and the electrolyte between cathode and anode, its
It is characterized in that：Electrolyte uses above-mentioned solid polymer electrolyte, and cathode includes：Positive electrode active materials, collector, conductive agent
And binding agent；Anode includes negative active core-shell material, collector, conductive agent and binding agent.
The all-solid lithium-ion battery, it is characterised in that the positive electrode active materials include：Cobalt acid lithium, LiMn2O4,
LiFePO4, lithium-nickel-cobalt-oxygen, lithium nickel cobalt manganese oxygen, lithium ferric manganese phosphate.
Embodiment 1
At ambient temperature by 0.36g LiTFSI, 0.2g PTMC (Mn=10000) and 0.8g PCL (Mn=
40000) it is dissolved in 30mL acetonitriles, stirring is transferred in Teflon mould to after forming uniform solution, then in air blast
With 70 DEG C of dry 16h in drying box, it is then transferred in vacuum drying chamber with 60 DEG C of dry 16h, obtains solid electrolyte film.
Solid electrolyte film is punched into after 16mm disks be transferred in the glove box of inert atmosphere place one day it is stand-by.Using phosphoric acid
Iron lithium assembles solid lithium battery, with 5mAg-1Multiplying power carry out loop test at room temperature.
Embodiment 2
At ambient temperature by 0.15gLiClO4, 0.2g PTMC (Mn=50000) and 0.8g PCL (Mn=50000)
It is dissolved in 30mL acetonitriles, stirring is transferred in Teflon mould to after forming uniform solution, then in air dry oven
In with 70 DEG C of dry 16h, be then transferred in vacuum drying chamber with 60 DEG C of dry 16h, obtain solid electrolyte film.By solid-state
Electrolytic thin-membrane be punched into after 16mm disks be transferred in the glove box of inert atmosphere place one day it is stand-by.Using lithium ferric manganese phosphate
Solid lithium battery is assembled, with 10mA g-1Multiplying power carry out loop test at room temperature.
Embodiment 3
At ambient temperature by 0.40g LiPF6, 0.2g PTMC (Mn=100000) and 0.8g PCL (Mn=
60000) it is dissolved in 30mL acetonitriles, stirring is transferred in Teflon mould to after forming uniform solution, then in air blast
With 70 DEG C of dry 16h in drying box, it is then transferred in vacuum drying chamber with 60 DEG C of dry 16h, obtains solid electrolyte film.
Solid electrolyte film is punched into after 16mm disks be transferred in the glove box of inert atmosphere place one day it is stand-by.Using mangaic acid
Lithium assembles solid lithium battery, with 10mA g-1Multiplying power carry out loop test at room temperature.
Embodiment 4
At ambient temperature by 0.25g LiBF4, 0.2g PTMC (Mn=200000) and 0.8g PCL (Mn=
100000) it is dissolved in 30mL acetonitriles, stirring is transferred in Teflon mould to after forming uniform solution, then in air blast
With 70 DEG C of dry 16h in drying box, it is then transferred in vacuum drying chamber with 60 DEG C of dry 16h, obtains solid electrolyte film.
Solid electrolyte film is punched into after 16mm disks be transferred in the glove box of inert atmosphere place one day it is stand-by.Using mangaic acid
Lithium assembles solid lithium battery, with 10mA g-1Multiplying power carry out loop test at room temperature.
Finally it should be noted that the foregoing is only a preferred embodiment of the present invention, this hair is not limited to
Bright, although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it is still
It can modify to the technical solution described in previous embodiment, or equivalent substitution is carried out to which part.It is all in this hair
Within bright spirit and principle, any modification, equivalent replacement, improvement and so on, should be included in protection scope of the present invention
Within.Although above-mentioned be described the embodiment of the present invention with reference to attached drawing, not to the scope of the present invention
Limitation, those skilled in the art should understand that, on the basis of technical scheme, those skilled in the art are not required to
The various modifications that can be made or deformation are made the creative labor still within protection scope of the present invention.
Claims (10)
- A kind of 1. solid polymer electrolyte, it is characterised in that the electrolyte by with lead lithium ion ability polymer and Lithium salts；Wherein, it is described have lead the polymer of lithium ion ability as the mixed of polytrimethylene carbonate PTMC and polycaprolactone (PCL) Compound.
- 2. electrolyte as claimed in claim 1, it is characterised in that the polytrimethylene carbonate and the quality of polycaprolactone The ratio between be 0.05~5：1.
- 3. electrolyte as claimed in claim 1, it is characterised in that in the electrolyte mass fraction of lithium salts for 10%~ 50%, it is 50%~90% with the mass fraction of the polymer of lithium ion ability in the electrolyte is led.
- 4. electrolyte as claimed in claim 1, it is characterised in that the molecular weight of the polytrimethylene carbonate is 0.1 ten thousand ~20 ten thousand.
- 5. electrolyte as claimed in claim 1, it is characterised in that the molecular weight of the polycaprolactone is 20,000~120,000.
- 6. electrolyte as claimed in claim 1, it is characterised in that the lithium salts is LiTFSI, LiPF6、LiClO4、 LiAsF6、LiBF4、LiCH3SO3、LiCF3SO3、LiBO、LiN(CF3SO2)2At least one of.
- A kind of 7. preparation method of solid polymer electrolyte, it is characterised in that including：At ambient temperature, lithium salts, polytrimethylene carbonate PTMC and polycaprolactone (PCL) are dissolved in acetonitrile or acetone, mixed Close uniformly, through drying twice, up to solid electrolyte film.
- 8. the method for claim 7, it is characterised in that described dry twice concretely comprises the following steps：In air dry oven In with 70 DEG C of dry 12~24h, be then transferred in vacuum drying chamber with 60 DEG C of dry 8~16h.
- 9. a kind of all-solid lithium-ion battery, is made of cathode, anode and the electrolyte between cathode and anode, it is special Sign is：Electrolyte uses claim 1-6 any one of them solid polymer electrolytes, and cathode includes：Positive-active material Material, collector, conductive agent and binding agent；Anode includes negative active core-shell material, collector, conductive agent and binding agent.
- 10. all-solid lithium-ion battery as described in claim 9, it is characterised in that the positive electrode active materials include：Cobalt Sour lithium, LiMn2O4, LiFePO4, lithium-nickel-cobalt-oxygen, lithium nickel cobalt manganese oxygen, lithium ferric manganese phosphate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711447568.8A CN107994257A (en) | 2017-12-27 | 2017-12-27 | A kind of high-performance solid electrolyte and preparation method thereof |
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| CN201711447568.8A CN107994257A (en) | 2017-12-27 | 2017-12-27 | A kind of high-performance solid electrolyte and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108923064A (en) * | 2018-07-10 | 2018-11-30 | 山西长韩新能源科技有限公司 | A kind of solid macromolecule electrolyte and preparation method thereof and lithium ion secondary battery |
| CN108963335A (en) * | 2018-07-13 | 2018-12-07 | 苏州思达奇环保新材料有限公司 | A kind of degradable electrolyte and preparation method thereof and its application in high specific energy solid-state lithium-air battery |
| CN109888369A (en) * | 2019-03-07 | 2019-06-14 | 东北师范大学 | A kind of all solid state electrolyte and preparation method thereof and a kind of lithium battery |
| CN111430791A (en) * | 2020-03-22 | 2020-07-17 | 华南理工大学 | In-situ polymerization polycaprolactone-based all-solid-state electrolyte and preparation method and application thereof |
| CN113675465A (en) * | 2021-07-27 | 2021-11-19 | 华南理工大学 | Modified polycaprolactone-based polymer solid electrolyte, preparation method thereof and all-solid-state metal lithium battery |
| CN114447422A (en) * | 2022-01-24 | 2022-05-06 | 中国地质大学（武汉） | High-power composite solid electrolyte based on polycaprolactone self-repair and preparation method thereof |
-
2017
- 2017-12-27 CN CN201711447568.8A patent/CN107994257A/en active Pending
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| BING SUN,ET AL.: ""Polycarbonate-based solid polymer electrolytes for Li-ion batteries"", 《SOLID STATE IONICS》 * |
| JONAS MINDEMARK, ET AL.: ""Copolymers of trimethylene carbonate and ε-caprolactone as electrolytes for lithium-ion batteries"", 《POLYMER》 * |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108923064A (en) * | 2018-07-10 | 2018-11-30 | 山西长韩新能源科技有限公司 | A kind of solid macromolecule electrolyte and preparation method thereof and lithium ion secondary battery |
| CN108923064B (en) * | 2018-07-10 | 2020-10-02 | 山西长韩新能源科技有限公司 | Solid polymer electrolyte, preparation method thereof and lithium ion secondary battery |
| CN108963335A (en) * | 2018-07-13 | 2018-12-07 | 苏州思达奇环保新材料有限公司 | A kind of degradable electrolyte and preparation method thereof and its application in high specific energy solid-state lithium-air battery |
| CN109888369A (en) * | 2019-03-07 | 2019-06-14 | 东北师范大学 | A kind of all solid state electrolyte and preparation method thereof and a kind of lithium battery |
| CN109888369B (en) * | 2019-03-07 | 2020-08-25 | 东北师范大学 | All-solid-state electrolyte, preparation method thereof and lithium battery |
| CN111430791A (en) * | 2020-03-22 | 2020-07-17 | 华南理工大学 | In-situ polymerization polycaprolactone-based all-solid-state electrolyte and preparation method and application thereof |
| CN111430791B (en) * | 2020-03-22 | 2021-08-06 | 华南理工大学 | In-situ polymerization polycaprolactone-based all-solid-state electrolyte and preparation method and application thereof |
| CN113675465A (en) * | 2021-07-27 | 2021-11-19 | 华南理工大学 | Modified polycaprolactone-based polymer solid electrolyte, preparation method thereof and all-solid-state metal lithium battery |
| CN114447422A (en) * | 2022-01-24 | 2022-05-06 | 中国地质大学（武汉） | High-power composite solid electrolyte based on polycaprolactone self-repair and preparation method thereof |
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