CN110247112A - A kind of high wettability sulfide based composite electrolyte and the preparation method and application thereof of " sandwich " structure - Google Patents
A kind of high wettability sulfide based composite electrolyte and the preparation method and application thereof of " sandwich " structure Download PDFInfo
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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
- 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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
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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
- H01M2300/0068—Solid electrolytes inorganic
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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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- 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
- H01M2300/0088—Composites
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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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of high wettability sulfide based composite electrolytes and the preparation method and application thereof of " sandwich " structure, and the composite electrolyte is by solid polyelectrolyte, sulfide solid electrolyte and solid polyelectrolyteIt is combined, in which: solid polyelectrolyte I improves interfacial wettability of the sulfide due to caused by space charge layer between positive electrode, improve electrochemical stability of the positive electrode in charge and discharge process for contacting with positive electrode；Solid polyelectrolyteFor contacting with lithium an- ode, the wetability between sulfide and negative electrode material is on the one hand improved, on the other hand inhibits the growth in metal negative electrode surface Li dendrite.Sulfide based composite electrolyte of the invention not only ionic conductivity with higher also has preferable interfacial wettability and stability.The present invention, which designs and optimizes for solid electrolyte material, provides new thinking, is conducive to the further development and commercialization of all-solid-state battery.
Description
Technical field
The invention belongs to all-solid-state battery technical field, be related to a kind of sulfide based composite electrolyte and preparation method thereof with
Using a kind of, and in particular to high wettability sulfide based composite electrolyte of " sandwich " structure and preparation method thereof and complete
Application in solid state battery.
Background technique
With the excessive use of the traditional fossil energies such as coal, petroleum, energy crisis, environmental pollution and ecological problem etc. are asked
Topic highlights.Lithium ion battery have energy density height, output power, voltage height, self discharge is small, operating temperature range is wide, nothing
Memory effect and advantages of environment protection are considered as most competitive one of electrochemical energy storage technology, and in each ring of energy storage
The application of section is also more and more extensive.But conventional lithium ion battery uses liquid state organic electrolyte as electrolyte, unavoidably
There are some problems, such as: the high reaction activity of lithium metal and organic electrolyte forms unstable SEI in metal surface
Film causes the reduction of active lithium, and electrolyte persistently exhausts, and reduces the capacity of battery and high rate performance；In addition to this, lithium metal
Nonuniform deposition be formed by Li dendrite and may pierce through diaphragm, cause battery short circuit, explosion occur etc..Solid electrolyte replaces
Liquid electrolyte is presently considered to be the ultimate method that can solve the above problem, and therefore, development has high-energy density, high safety
The all-solid lithium-ion battery of property or even high power density is only selection.
And the core of solid lithium battery technology is electrolyte, solid state electrolysis Quality Research is concentrated mainly on poly- at present
Polymer electrolyte, oxide electrolyte and sulfide electrolyte.Wherein oxide electrolyte have preferable thermal stability and
Chemical compatibility, but how to improve lithium ion conduction ability at room temperature and improve interface compatibility become one it is severe
Challenge.Polymer dielectric is made of polymeric matrix and lithium salts, has many advantages, such as that viscoelasticity is good, machining property is excellent,
But ionic conductivity at room temperature is low；And sulfide electrolyte causes distortion of lattice since the atomic radius and polarizability of S are big
Biggish ion channel is formed, shows preferable ionic conductance, but sulfide electrolyte is extremely unstable in air, removes
Except this, since the presence of space charge layer makes the interfacial contact of sulfide not be fine.Based on the above various electrolyte
Advantage and disadvantage and solid electrolyte there are the problem of, be highly desirable to invent a kind of not only stable, but also have good interface compatible
Polymer/sulfide/composites polymer electrolytes of property and high ionic conductivity.
Summary of the invention
Based on above technical background, the present invention provides a kind of structure novels, easy to operate, " Sanming City for haveing excellent performance
Control " the high wettability sulfide based composite electrolyte and the preparation method and application thereof of structure.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of high wettability sulfide based composite electrolyte of " sandwich " structure, it is solid by solid polyelectrolyte, sulfide
State electrolyte and solid polyelectrolyteIt is combined.As shown in Figure 1, polymer dielectric I with positive electrode for connecing
Touching improves interfacial wettability of the sulfide due to caused by space charge layer between positive electrode, improves positive electrode and is filling
Electrochemical stability in discharge process；On the one hand solid polyelectrolyte improves vulcanization for contacting with lithium an- ode
On the other hand wetability between object and negative electrode material inhibits the growth in metal negative electrode surface Li dendrite.
A kind of preparation method of the high wettability sulfide based composite electrolyte of above-mentioned " sandwich " structure, including walk as follows
It is rapid:
Step 1: the preparation of sulfide electrolyte
(1) sulfide solid electrolyte is subjected to 0.5 ~ 3h of heat treatment at a high temperature of 240 ~ 280, then grinding obtains solid-state electricity
Solve matter powder, in which: the sulfide solid electrolyte is selected from Li4-xGe1-xPxS2(1-x)(x=0.55~1)、 Li2S-Al2S3-
P2S5、8Li3PS413.1LiAlS2、 Li2S-P2S5-LiI、Li2S-P2S5-LiBr、Li2S-P2S5-LiBH4、 Li2S-P2S5-
Ge0.35Ga0.05Se0.60、67Li2S-33P2S5、75Li2S-25P2S5(Li3PS4), 70Li2S-30P2S5(Li7P3S11)、70
(0.75Li2S-0.25P2S5)-30MgO、70(0.75Li2S-0.25P2S5)-30Li2O、70(0.75Li2S-0.25P2S5)-30CaO、
70(0.75Li2S-0.25P2S5)-30CuO、70(0.75Li2S-0.25P2S5)-30FeS、75LiS-15P2S5-10P2O5In
It is a kind of；
(2) solid electrolyte powder is pressed into solid electrolyte piece in glove box, can be obtained sulfide solid electrolyte piece；
Step 2: solid polyelectrolyte solutionPreparation
(1) by polymerBe dissolved in suitable acetonitrile solution with lithium salts, at room temperature stir 10 ~ for 24 hours, obtain polymer electrolytic
Matter solution, in which: the polymerSelected from Pluronic F-127 (PEO), polyacrylonitrile (PAN), polyvinyl alcohol (PVA), gather partially
One of vinyl fluoride (PVDF), polymethyl methacrylate (PMMA), polyethylene glycol；The polymerWith mole of lithium salts
Than for 10 ~ 20:1；The lithium salts is one of dioxalic acid lithium borate LiBOB, difluorine oxalic acid boracic acid lithium LiODFB；
Step 3: the preparation of solid polyelectrolyte
By polymerBe dissolved in suitable acetonitrile solution with lithium salts, at room temperature stir 10 ~ for 24 hours, obtain polymer dielectric
Solution, in which: the polymerSelected from Pluronic F-127 (PEO), polyacrylonitrile (PAN), polyvinyl alcohol (PVA), gather inclined fluorine
One of ethylene (PVDF), polymethyl methacrylate (PMMA), polyethylene glycol；The molar ratio of polymer and lithium salts be 10 ~
20:1；The lithium salts is lithium nitrate LiNO3, one of lithium fluoride LiF；
Step 4: the preparation of " sandwich " structure sulfide based composite electrolyte
Method one:
(1) by solid polyelectrolyte solutionCoated in sulfide solid electrolyte piece surface, vacuum drying；
(2) in the other side coated polymer solid electrolyte of sulfide solid electrolyte piece, can be obtained after vacuum drying
Solid polyelectrolyte/ sulfide solid electrolyte/solid polyelectrolyteThe composite electrolyte of structure, in which: sulphur
Compound solid electrolyte with a thickness of 300 ~ 600 μm, solid polyelectrolyteAnd solid polyelectrolyteWith a thickness of
30 ~ 150 μm, the above operation carries out in glove box；
Method two:
Solid polyelectrolyte solution and solid polyelectrolyte solution are dried at room temperature for 12 ~ for 24 hours, then 50 ~
At 70 DEG C vacuum drying 12 ~ for 24 hours, the solid polyelectrolyte of acquisition and solid polyelectrolyte are subjected to hot pressing respectively,
Cut-parts.Operation order during assembling all-solid-state battery is anode cover/positive electrode/polymer dielectric I/ sulfide electricity
Solve matter/polymer dielectric/ lithium piece/gasket/elastic slice/negative electrode casing, obtained electrolyte portion is " sandwich " at this time
The composite electrolyte of structure, in which: sulfide solid electrolyte with a thickness of 300 ~ 600 μm, solid polyelectrolyteWith it is poly-
Close object solid electrolyteThickness control at 30 ~ 150 μm;Wherein: the anode includes NCM(622), NCM(811) ternary material
Material, any one in LiFePO 4 material.
Compared with the prior art, the present invention has the advantage that
1, sulfide electrolyte is contacted by polymer dielectric with positive electrode, negative metal lithium in the present invention, improves boundary
The wetability and compatibility in face.
2, the polymer dielectric used in the present inventionIt is steady to improve electrochemistry of the positive electrode in charge and discharge process
It is qualitative.
3, polymer dielectric used in present invention instituteInhibit the growth in lithium anode surface dendrite.
4, sulfide based composite electrolyte of the invention not only ionic conductivity with higher also has preferable interface
Wetability and stability.
5, the present invention, which designs and optimized for solid electrolyte material, provides a kind of new thinking, is conducive to all-solid-state battery
It is further development and commercialization.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the high wettability sulfide based composite electrolyte of " sandwich " structure of the invention, in figure:
1- negative electrode casing, 2- elastic slice, 3- gasket, 4- lithium piece, 5- electrolyte, 6- positive plate, 7- anode cover, 8- solid polyelectrolyte
, 9- sulfide solid electrolyte, 10- solid polyelectrolyte。
Fig. 2 is the one lateral inhibition Li dendrite of high wettability sulfide based composite electrolyte cathode of " sandwich " structure of the invention
The schematic diagram of growth.
Specific embodiment
Below with reference to embodiment, further description of the technical solution of the present invention, and however, it is not limited to this, all right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be contained
Lid is within the protection scope of the present invention.
Embodiment 1
The preparation step of the high wettability sulfide based composite electrolyte of " sandwich " structure provided in this embodiment is as follows:
(1) by Li2S and P2S5High-energy ball milling is carried out according to the molar ratio of 70:30, obtains the higher Li of ionic conductivity7P3S11's
Sulfide solid electrolyte.
(2) the sulfide solid electrolyte obtained in step (1) is subjected to heat treatment 1h at a high temperature of 240 DEG C, then
Grinding obtains solid electrolyte powder.
(3) solid electrolyte powder is pressed into sulfide solid electrolyte piece in glove box.
(4) Kynoar and dioxalic acid lithium borate LiBOB are dissolved according to the ratio that molar ratio is 10:1 suitable
In acetonitrile solution, 10h is stirred at room temperature, obtains polyelectrolyte solution I.
(5) by Kynoar and lithium nitrate LiNO3It is molten that suitable acetonitrile is dissolved according to the ratio that molar ratio is 10:1
In liquid, 10h is stirred at room temperature, obtains polyelectrolyte solution II.
(6) polyelectrolyte solution I is coated in the sulfide bath surface suppressed, is being vulcanized after vacuum drying
The other side coated polymer electrolyte solution II of object electrolyte, can be obtained polymer/sulfide/polymer after vacuum drying
The composite electrolyte of structure, in which: sulfide electrolyte with a thickness of 500 μm, solid polyelectrolyteAnd polymer solid
ElectrolyteWith a thickness of 50 μm, the above operation carries out in gloves molding box.
Embodiment 2
(1) by Li2S and P2S5High-energy ball milling is carried out according to the molar ratio of 75:25, obtains the higher Li of ionic conductivity3PS4's
Sulfide solid electrolyte.
(2) the sulfide solid electrolyte obtained in step (1) is subjected to heat treatment 1h at a high temperature of 260 DEG C, then
Grinding obtains solid electrolyte powder.
(3) solid electrolyte powder is pressed into sulfide solid electrolyte piece in glove box.
(4) polyethylene glycol oxide and difluorine oxalic acid boracic acid lithium LiODFB are dissolved in right amount according to the ratio that molar ratio is 18:1
Acetonitrile solution in, stir at room temperature for 24 hours, obtain polyelectrolyte solution I.
(5) by polyethylene glycol oxide (PEO) and lithium nitrate LiNO3Suitable second is dissolved according to the ratio that molar ratio is 18:1
In nitrile solution, stirs at room temperature for 24 hours, obtain polyelectrolyte solution。
(6) by polyelectrolyte solution I and polyelectrolyte solutionIt is dried at room temperature for 12h, then at 60 DEG C
It is lower to be dried in vacuo for 24 hours, by the solid solid polyelectrolyte of acquisitionAnd solid polyelectrolyteHot pressing is carried out respectively, is cut out
Piece.
(7) operation order is anode cover/positive electrode/polymer dielectric I/ vulcanization during assembling all-solid-state battery
Object electrolyte/polyelectrolyte solution/ lithium piece/gasket/elastic slice/negative electrode casing (Fig. 1), in which: the thickness of sulfide electrolyte
Degree is 400 μm, solid polyelectrolyteAnd solid polyelectrolyteThickness control at 80 μm.
Claims (10)
1. a kind of high wettability sulfide based composite electrolyte of " sandwich " structure, it is characterised in that the composite electrolyte by
Solid polyelectrolyte, sulfide solid electrolyte and solid polyelectrolyteIt is combined.
2. the high wettability sulfide based composite electrolyte of " sandwich " structure according to claim 1, it is characterised in that
The sulfide solid electrolyte is selected from Li4-xGe1-xPxS2(1-x)、 Li2S-Al2S3-P2S5、8Li3PS413.1LiAlS2、 Li2S-
P2S5-LiI、Li2S-P2S5-LiBr、Li2S-P2S5-LiBH4、 Li2S-P2S5-Ge0.35Ga0.05Se0.60、67Li2S-33P2S5、
75Li2S-25P2S5、70Li2S-30P2S5、70(0.75Li2S-0.25P2S5)-30MgO、70(0.75Li2S-0.25P2S5)-
30Li2O、70(0.75Li2S-0.25P2S5)-30CaO、70(0.75Li2S-0.25P2S5)-30CuO、70(0.75Li2S-
0.25P2S5)-30FeS、LiPS4、75LiS-15P2S5-10P2O5One of, x=0.55 ~ 1.
3. a kind of preparation side of the high wettability sulfide based composite electrolyte of " sandwich " structure of any of claims 1 or 2
Method, it is characterised in that described method includes following steps:
Step 1: the preparation of sulfide electrolyte
(1) sulfide solid electrolyte is subjected to 0.5 ~ 3h of heat treatment at a high temperature of 240 ~ 280, then grinding obtains solid-state electricity
Solve matter powder；
(2) solid electrolyte powder is pressed into solid electrolyte piece in glove box, can be obtained sulfide solid electrolyte；
Step 2: solid polyelectrolyte solutionPreparation
(1) by polymerBe dissolved in acetonitrile solution with lithium salts, at room temperature stir 10 ~ for 24 hours, obtain polyelectrolyte solution；
Step 3: solid polyelectrolytePreparation
By polymerBe dissolved in acetonitrile solution with lithium salts, at room temperature stir 10 ~ for 24 hours, obtain polyelectrolyte solution；
Step 4: the preparation of " sandwich " structure sulfide based composite electrolyte
(1) by solid polyelectrolyte solutionCoated in sulfide solid electrolyte surface, vacuum drying；
(2) in the other side coated polymer solid electrolyte of sulfide solid electrolyte, can be obtained polymerization after vacuum drying
Object solid electrolyte/ sulfide solid electrolyte/solid polyelectrolyteThe composite electrolyte of structure.
4. the preparation method of the high wettability sulfide based composite electrolyte of " sandwich " structure according to claim 3,
It is characterized in that the polymerAnd polymerSelected from Pluronic F-127, polyacrylonitrile, polyvinyl alcohol, Kynoar, gather
One of methyl methacrylate, polyethylene glycol.
5. the preparation side of the high wettability sulfide based composite electrolyte of " sandwich " structure according to claim 3 or 4
Method, it is characterised in that the polymerMolar ratio with lithium salts is 10 ~ 20:1；The lithium salts be dioxalic acid lithium borate LiBOB,
One of difluorine oxalic acid boracic acid lithium LiODFB.
6. the preparation side of the high wettability sulfide based composite electrolyte of " sandwich " structure according to claim 3 or 4
Method, it is characterised in that the molar ratio of the polymer and lithium salts is 10 ~ 20:1；The lithium salts is lithium nitrate LiNO3, lithium fluoride
One of LiF.
7. the preparation method of the high wettability sulfide based composite electrolyte of " sandwich " structure according to claim 3,
It is characterized in that the step 4 replacement are as follows: by solid polyelectrolyte solutionWith solid polyelectrolyte solution in room
Temperature lower dry 12 ~ for 24 hours, the then vacuum drying 12 ~ for 24 hours at 50 ~ 70 DEG C, by the solid solid polyelectrolyte of acquisitionWith it is poly-
Close object solid electrolyteHot pressing, cut-parts are carried out respectively.
8. the preparation side of the high wettability sulfide based composite electrolyte of " sandwich " structure according to claim 3 or 7
Method, it is characterised in that the sulfide solid electrolyte with a thickness of 300 ~ 600 μm, solid polyelectrolyteAnd polymer
Solid electrolyteThickness control at 30 ~ 150 μm.
9. a kind of high wettability sulfide based composite electrolyte of " sandwich " structure as claimed in claim 1 or 2 is in all solid state electricity
Application in pond.
10. the high wettability sulfide based composite electrolyte of " sandwich " structure according to claim 9 is in all solid state electricity
Application in pond, it is characterised in that the assemble sequence of the all-solid-state battery is anode cover/positive electrode/polymer dielectric I/
Sulfide electrolyte/polyelectrolyte solution/ lithium piece/gasket/elastic slice/negative electrode casing.
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| CN111933999B (en) * | 2020-09-15 | 2021-03-26 | 江苏时代新能源科技有限公司 | Solid-state battery, battery module, battery pack and related device thereof |
| WO2022057189A1 (en) * | 2020-09-15 | 2022-03-24 | 江苏时代新能源科技有限公司 | Solid-state battery, battery module, battery pack, and related device thereof |
| WO2022104929A1 (en) * | 2020-11-23 | 2022-05-27 | 瑞声声学科技(深圳)有限公司 | Composite sulfide solid electrolyte, battery and preparation method therefor |
| CN112820935A (en) * | 2020-12-31 | 2021-05-18 | 长三角物理研究中心有限公司 | Novel battery based on sulfide solid electrolyte |
| CN112820934A (en) * | 2021-02-09 | 2021-05-18 | 苏州清陶新能源科技有限公司 | Solid-state lithium ion battery and charging protection method based on solid-state lithium ion battery |
| WO2022222894A1 (en) * | 2021-04-19 | 2022-10-27 | 华为技术有限公司 | Metal negative electrode, battery, and electronic device |
| CN116315076A (en) * | 2023-05-22 | 2023-06-23 | 西北工业大学 | Solid electrolyte with continuous ion transmission path, and preparation method and application thereof |
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