CN109698381A - A kind of carbon-based boundary layer of solid electrolyte and its preparation method and application - Google Patents
A kind of carbon-based boundary layer of solid electrolyte and its preparation method and application Download PDFInfo
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- CN109698381A CN109698381A CN201710990899.XA CN201710990899A CN109698381A CN 109698381 A CN109698381 A CN 109698381A CN 201710990899 A CN201710990899 A CN 201710990899A CN 109698381 A CN109698381 A CN 109698381A
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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
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M2300/0071—Oxides
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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
- H01M2300/0094—Composites in the form of layered products, e.g. coatings
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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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Abstract
The present embodiments relate to carbon-based boundary layer of a kind of solid electrolyte and its preparation method and application, carbon-based boundary layer is on the surface that solid electrolyte is in contact with the alkali metal cathode of battery；Carbon-based boundary layer is the composite material of carbon material or carbon-based material or the carbon material and the carbon-based material；Wherein, carbon material includes: one of natural graphite, electrographite, graphite microchip, acetylene black, carbon nanotube, carbon fiber, graphene, graphene oxide, redox graphene or amorphous carbon or a variety of；Carbon-based material include: containing alkyl, hydroxyl, carboxyl, carbonyl, cyano, alkenyl, alkynyl organic group carbon-based material.
Description
Technical field
The present invention relates to field of material technology more particularly to a kind of carbon-based boundary layer of solid electrolyte and preparation method thereof
And application.
Background technique
With domestic economy fast development, the role of battery in people's daily life is more and more important.Traditional lithium from
Sub- battery is now widely used for miniaturized electronics, but its liquid state organic electrolyte system is inflammable, and there are security risk, systems
About it is further in the application in extensive energy storage field and power battery field.Develop next-generation high-energy density, Gao An
Full property battery has become the research hotspot of every country, and exploitation novel battery is very urgent.
Solid state battery is considered as most promising next-generation battery system.Solid state battery replaces tradition with solid electrolyte
Diaphragm electrolysis liquid system in lithium ion battery, solve lithium ion battery security risk (Nature, 2008,451
(7179): 652-657, Nature, 2001,414 (6861): 359-367).Meanwhile solid state battery can be used alkali metal and bear
Pole greatly improves the energy density of battery system, has greatly expanded its application field.But solid state cell technology is also deposited at present
In great number of issues, wherein the compatibility of solid electrolyte and alkali metal cathode is one of main problem.For this purpose, proposing in the industry solid
The boundary layers such as aluminium oxide, silicon, germanium, gold, but such boundary layer expensive starting materials are introduced between body electrolyte and alkali metal, and need to pass through
Depositional mode is prepared (atomic layer deposition, vapor deposition, magnetron sputtering etc.), complicated for operation, and equipment is expensive, it is difficult to answer on a large scale
With.Therefore, it is necessary to develop a kind of low in raw material price, the simple New Solid electrolyte interface layer of preparation method improves solid-state
The compatibility of electrolyte and alkali metal pushes the development of solid state battery.
Summary of the invention
The object of the present invention is to provide carbon-based boundary layers of a kind of solid electrolyte and its preparation method and application, pass through carbon
The interface resistance of base boundary layer reduction solid electrolyte and alkali metal.
To achieve the above object, described in a first aspect, the present invention provides a kind of carbon-based boundary layer of solid electrolyte
Carbon-based boundary layer is on the surface that the solid electrolyte is in contact with the alkali metal cathode of battery；The carbon-based boundary layer is carbon
The composite material of material or carbon-based material or the carbon material and the carbon-based material；
Wherein, the carbon material includes: natural graphite, electrographite, graphite microchip, acetylene black, carbon nanotube, carbon fiber
One of dimension, graphene, graphene oxide, redox graphene or amorphous carbon are a variety of；The carbon-based material includes:
Containing alkyl, hydroxyl, carboxyl, carbonyl, cyano, alkenyl, alkynyl organic group carbon-based material.
Preferably, the carbon-based boundary layer with a thickness of 1nm~1 μm.
Preferably, the solid electrolyte is lithium ion conductor or sodium ion conductor；
Wherein, the lithium ion conductor include: garnet Garnet type structure oxide, NASICON type structure oxide,
LISICON type structure oxide, LISICON type structure sulfide or perovskite structure oxide；
The sodium ion conductor includes: NASICON type structure oxide or perovskite structure oxide.
Preferably, the alkali metal includes: any one of lithium metal, metallic sodium, lithium metal alloy or metal sodium alloy.
Preferably, the organic group include: one of alkyl, hydroxyl, carboxyl, carbonyl, cyano, alkenyl, alkynyl or
It is several.
In second aspect, the embodiment of the invention provides a kind of preparation sides of carbon-based boundary layer described in above-mentioned first aspect
Method, the preparation method is that Mechanical Method, comprising:
The surface of polishing solid electrolyte sheet；
The carbon material of solid or the composite material of carbon-based material or the carbon material and the carbon-based material are taken, in institute
It states surface and carries out mechanical friction, directly form the carbon-based boundary layer；
Wherein, the carbon material includes: natural graphite, electrographite, graphite microchip, acetylene black, carbon nanotube, carbon fiber
One of dimension, graphene, graphene oxide, redox graphene or amorphous carbon are a variety of；The carbon-based material includes:
Containing alkyl, hydroxyl, carboxyl, carbonyl, cyano, alkenyl, alkynyl organic group carbon-based material.
In the third aspect, the embodiment of the invention provides a kind of preparation sides of carbon-based boundary layer described in above-mentioned first aspect
Method, the preparation method is that solution spin-coating method, comprising:
The surface of polishing solid electrolyte sheet；
The composite material of carbon material or carbon-based material or the carbon material and the carbon-based material is dissolved in solvent, shape
At solution；
The solution is spin-coated on to the surface of the solid electrolyte sheet using spin coater, forms the carbon-based boundary layer；
Wherein, the carbon material includes: natural graphite, electrographite, graphite microchip, acetylene black, carbon nanotube, carbon fiber
One of dimension, graphene, graphene oxide, redox graphene or amorphous carbon are a variety of；The carbon-based material includes:
Containing alkyl, hydroxyl, carboxyl, carbonyl, cyano, alkenyl, alkynyl organic group carbon-based material；The solvent is water, You Jirong
Agent or ionic liquid.
Preferably, the concentration of the solution is 0.01mol/L~10mol/L.
Fourth aspect, the embodiment of the invention provides a kind of solid electrolytes, have carbon-based described in above-mentioned first aspect
Boundary layer.
5th aspect, the embodiment of the invention provides a kind of batteries, including solid electrolyte described in above-mentioned fourth aspect.
The carbon-based boundary layer of solid electrolyte provided in an embodiment of the present invention is the pass in New Solid cell manufacturing process
Key technology, preparation method is simple, the interface resistance of solid electrolyte and alkali metal can be effectively reduced, and prepared by raising
The energy density and power density of solid state battery, have a extensive future.
Detailed description of the invention
Fig. 1 is untreated Garnet structure lithium ion conductive ceramic piece provided in an embodiment of the present invention, and lithium metal is symmetrically electric
Pond electrochemical impedance spectroscopy；
Fig. 2 is that carbon-based boundary layer provided in an embodiment of the present invention handles Garnet structure lithium ion conductive ceramic piece, metal
Lithium Symmetrical cells electrochemical impedance spectroscopy；
Fig. 3 is the comparison diagram of two electrochemical impedance spectroscopies of Fig. 1 provided in an embodiment of the present invention and Fig. 2；
Fig. 4 is untreated NASICON structure sodium ion conductor potsherd provided in an embodiment of the present invention, and metallic sodium is symmetrically electric
Pond electrochemical impedance spectroscopy；
Fig. 5 is that carbon-based boundary layer provided in an embodiment of the present invention handles NASICON structure sodium ion conductor potsherd, metal
Sodium Symmetrical cells electrochemical impedance spectroscopy.
Specific embodiment
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
The carbon-based boundary layer of solid electrolyte provided in an embodiment of the present invention, it is negative in the alkali metal of solid electrolyte and battery
On the surface that pole is in contact, with a thickness of 1nm~1 μm.Carbon-based boundary layer is specially carbon material perhaps carbon-based material or above-mentioned carbon
The composite material of material and carbon-based material.
Above-mentioned carbon material may include: natural graphite, electrographite, graphite microchip, acetylene black, carbon nanotube, carbon fiber,
One of graphene, graphene oxide, redox graphene or amorphous carbon etc. are a variety of；Carbon-based material may include:
Carbon-based material containing organic groups such as alkyl, hydroxyl, carboxyl, carbonyl, cyano, alkenyl, alkynyls, wherein organic group can wrap
It includes: one or more of alkyl, hydroxyl, carboxyl, carbonyl, cyano, alkenyl, alkynyl etc..
Above-mentioned solid electrolyte can be specially lithium ion conductor or sodium ion conductor；Wherein, lithium ion conductor includes: stone
Garnet (Garnet) type structure oxide, NASICON type structure oxide, LISICON type structure oxide, LISICON type knot
Structure sulfide or perovskite structure oxide；Sodium ion conductor includes: NASICON type structure oxide or perovskite structure oxidation
Object.
Alkali metal may include: any one of lithium metal, metallic sodium, lithium metal alloy or metal sodium alloy.
Carbon-based boundary layer is located at the surface that solid electrolyte is in contact with the alkali metal cathode of battery, can be effectively reduced solid
The interface resistance of body electrolyte and alkali metal improves the energy density and power density of prepared solid state battery, is novel solid
Key technology in state cell manufacturing process, has a extensive future.
The carbon-based boundary layer of solid electrolyte provided in an embodiment of the present invention can be prepared by a variety of methods, below
It is illustrated respectively by taking Mechanical Method and solution spin-coating method as an example.
Carbon-based boundary layer is prepared using Mechanical Method:
Solid electrolyte sheet is taken to carry out surface polishing with sand paper.Take above-mentioned carbon material, carbon-based material or the composite wood of solid
Material, is polished a side surface in solid electrolyte sheet and gently rubs, carbon-based boundary layer is prepared.
Carbon-based boundary layer is prepared using solution spin-coating method:
Solid electrolyte sheet is taken to carry out surface polishing with sand paper.Above-mentioned carbon material, carbon-based material or composite material are dissolved in
Corresponding solvent, such as: water, organic solvent or ionic liquid are configured to 0.01mol/L~10mol/L solution, reuse spin coating
Machine is polished a side surface in solid electrolyte sheet and coats, and vacuumizing and drying forms carbon-based boundary layer.
In a specific example, 50wt% alcohol water blend, solution concentration 1mol/L, drying temperature can be used
It is 120 DEG C.
Carbon-based boundary layer and preparation method thereof is described above, is applied to below and performance is illustrated.
Carbon-based boundary layer of the invention is applied to the boundary layer of the solid electrolyte of battery, will have the carbon-based boundary layer
Solid electrolyte is assembled into battery and performance test is as follows:
2025 button cells are prepared, electrification is carried out to the battery of the solid electrolyte with the carbon-based boundary layer of the invention
Learn impedance spectrum test.Specific installation step is that alkali metal is made to diameter 1mm, 300 μm of disks of thickness, is affixed on solid electrolyte pottery
Tile two sides is packaged in button cell shell, carries out ac impedance spectroscopy test.Frequency range 10Mhz-10mHz.
With Garnet type lithium ion conductor Li7La3Zr2O12Potsherd is carried out as solid electrolyte according to above-mentioned Mechanical Method
Interface processing obtains carbon-based boundary layer.And it is compared with untreated potsherd.Using lithium metal as alkali metal, referring to above-mentioned
The preparation process of 2025 button cells prepares button cell, tests AC impedance, untreated Garnet structure lithium ion conductor pottery
Tile, lithium metal Symmetrical cells electrochemical impedance spectroscopy is as shown in Figure 1, carbon-based boundary layer processing Garnet structure lithium ion conductor pottery
Tile, lithium metal Symmetrical cells electrochemical impedance spectroscopy are as shown in Figure 2.For the ease of comparison, we are by two kinds of electricity of Fig. 1 and Fig. 2
Chemical impedance spectrum superposition forms Fig. 3, to intuitively see the comparison handled by carbon-based boundary layer with untreated interface.
With NASICON type sodium ion conductor Na3Zr2Si2PO12Potsherd is as solid electrolyte, according to above-mentioned solution spin coating
Method carries out interface processing, obtains carbon-based boundary layer.And it is compared with untreated potsherd.Using metallic sodium as alkali metal, reference
The preparation process of above-mentioned 2025 button cell prepares button cell, tests AC impedance, and untreated NASICON structure sodium ion is led
Body potsherd, metallic sodium Symmetrical cells electrochemical impedance spectroscopy is as shown in figure 4, carbon-based boundary layer handles NASICON structure sodium ion
Conductive ceramic piece, metallic sodium Symmetrical cells electrochemical impedance spectroscopy are as shown in Figure 5.
It can be seen that by the comparison of Fig. 3 and Fig. 4, Fig. 5 using carbon-based boundary layer provided by the invention, solid electrolytic
The interface resistance of matter and alkali metal is smaller, therefore solid state battery can obtain higher energy density and power density, to battery
Performance boost play a key effect.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not intended to limit the present invention the foregoing is merely a specific embodiment of the invention
Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (9)
1. a kind of carbon-based boundary layer of solid electrolyte, which is characterized in that the carbon-based boundary layer the solid electrolyte with
On the surface that the alkali metal cathode of battery is in contact；The carbon-based boundary layer is carbon material or carbon-based material or the carbon materials
The composite material of material and the carbon-based material；
Wherein, the carbon material includes: natural graphite, electrographite, graphite microchip, acetylene black, carbon nanotube, carbon fiber, stone
One of black alkene, graphene oxide, redox graphene or amorphous carbon are a variety of；The carbon-based material includes: containing alkane
Base, hydroxyl, carboxyl, carbonyl, cyano, alkenyl, alkynyl organic group carbon-based material.
2. carbon-based boundary layer according to claim 1, which is characterized in that the carbon-based boundary layer with a thickness of the μ of 1nm~1
m。
3. carbon-based boundary layer according to claim 1, which is characterized in that the solid electrolyte is lithium ion conductor or sodium
Ion conductor；
Wherein, the lithium ion conductor include: garnet Garnet type structure oxide, NASICON type structure oxide,
LISICON type structure oxide, LISICON type structure sulfide or perovskite structure oxide；
The sodium ion conductor includes: NASICON type structure oxide or perovskite structure oxide.
4. carbon-based boundary layer according to claim 1, which is characterized in that the alkali metal include: lithium metal, metallic sodium,
Any one of lithium metal alloy or metal sodium alloy.
5. a kind of preparation method of any carbon-based boundary layer of the claims 1-4, which is characterized in that the preparation method
For Mechanical Method, comprising:
The surface of polishing solid electrolyte sheet；
The carbon material of solid or the composite material of carbon-based material or the carbon material and the carbon-based material are taken, in the table
Face carries out mechanical friction, directly forms the carbon-based boundary layer；
Wherein, the carbon material includes: natural graphite, electrographite, graphite microchip, acetylene black, carbon nanotube, carbon fiber, stone
One of black alkene, graphene oxide, redox graphene or amorphous carbon are a variety of；The carbon-based material includes: containing alkane
Base, hydroxyl, carboxyl, carbonyl, cyano, alkenyl, alkynyl organic group carbon-based material.
6. a kind of preparation method of any carbon-based boundary layer of the claims 1-4, which is characterized in that the preparation method
For solution spin-coating method, comprising:
The surface of polishing solid electrolyte sheet；
The composite material of carbon material or carbon-based material or the carbon material and the carbon-based material is dissolved in solvent, is formed molten
Liquid；
The solution is spin-coated on to the surface of the solid electrolyte sheet using spin coater, forms the carbon-based boundary layer；
Wherein, the carbon material includes: natural graphite, electrographite, graphite microchip, acetylene black, carbon nanotube, carbon fiber, stone
One of black alkene, graphene oxide, redox graphene or amorphous carbon are a variety of；The carbon-based material includes: containing alkane
Base, hydroxyl, carboxyl, carbonyl, cyano, alkenyl, alkynyl organic group carbon-based material；The solvent be water, organic solvent or
Ionic liquid.
7. the preparation method of carbon-based boundary layer according to claim 6, which is characterized in that the concentration of the solution is
0.01mol/L~10mol/L.
8. a kind of solid electrolyte, which is characterized in that the solid electrolyte has any carbon of the claims 1-4
Base boundary layer.
9. a kind of battery, which is characterized in that the battery includes solid electrolyte described in the claims 8.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110085910A (en) * | 2019-05-14 | 2019-08-02 | 中南大学 | Solid lithium battery, garnet solid electrolyte and preparation method thereof |
| CN110098432A (en) * | 2019-06-03 | 2019-08-06 | 哈尔滨工业大学 | A kind of preparation method and applications of carbon fiber cladding solid electrolyte material |
| CN110444809A (en) * | 2019-08-14 | 2019-11-12 | 中国科学院宁波材料技术与工程研究所 | A kind of composite electrolyte piece and preparation method thereof and solid state battery |
| CN111653819A (en) * | 2020-06-09 | 2020-09-11 | 长沙矿冶研究院有限责任公司 | Solid-state battery and preparation method thereof |
| CN112786957A (en) * | 2019-11-05 | 2021-05-11 | 中天储能科技有限公司 | Polymer solid electrolyte, preparation method thereof and polymer solid battery |
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| CN111653819A (en) * | 2020-06-09 | 2020-09-11 | 长沙矿冶研究院有限责任公司 | Solid-state battery and preparation method thereof |
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