CN107863533A - A kind of Oxide electrolyte materials of glassy state - Google Patents
A kind of Oxide electrolyte materials of glassy state Download PDFInfo
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- CN107863533A CN107863533A CN201710914119.3A CN201710914119A CN107863533A CN 107863533 A CN107863533 A CN 107863533A CN 201710914119 A CN201710914119 A CN 201710914119A CN 107863533 A CN107863533 A CN 107863533A
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- H01M10/0561—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
- H01M10/056—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
- H01M10/0563—Liquid materials, e.g. for Li-SOCl2 cells
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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
- H01M2300/002—Inorganic electrolyte
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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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- 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
Abstract
The invention provides a kind of oxide solution matter of glassy state available for lithium battery, its chemical formula is LixM1yM2y’OzRepresent, wherein M1 be magnesium, aluminium, titanium, iron, copper, zinc, zirconium, tin, cerium, the one or more among lanthanum, and described M2 is boron, carbon, nitrogen, fluorine, silicon, phosphorus, the one or more among sulphur, described x, y, y ', z span be 1<X≤10,0≤y≤5,0≤y '≤3,0<Z≤12, wherein, when M1 is titanium and y '=0, x value is not equal to 2 or 4；When M1 is titanium elements, M2 can not take P element；As y=0, x value is not equal to 2 or 3.
Description
Technical field
The present invention relates to technical field of lithium ion.
Background technology
Lithium ion battery has been widely used for consumer electronics product, electricity as a kind of energy storage technology of high-energy-density
The field such as electrical automobile and extensive energy storage.
Lithium ion battery is mainly made up of positive pole, negative pole, barrier film and electrolyte.Wherein, anolyte portion is typically by easy
The organic solvent dissolving lithium salts of volatilization is made, and leakage and burning easily occurs, therefore larger potential safety hazard be present.When using non-
Volatile solid electrolyte substitutes the barrier film and anolyte portion in lithium ion battery, then it is higher can to obtain security performance
Solid state lithium battery.As can be seen here, solid electrolyte is the core of solid state lithium battery.
The main organic/inorganic substance of existing solid electrolyte and the major class of polymer two.Wherein, can be by nothing according to the structure of matter
Machine solid electrolyte is divided into crystal-type and amorphous build（Glassy state）Two kinds.Crystal-type electrolyte mainly includes perovskite, knot
Crystalline substance superionic conductors class, sodium superionic conductors class and stratiform Li3N classes；Amorphous build solid electrolyte mainly includes oxide
Glassy state and chalcogenide glass state and LIPON classes.
At present, the mainly chalcogenide glass state electrolyte with larger application prospect, such as 20th century are disclosed
LiI-Li2S-SiS2、Li3PO4-Li2S-SiS2（Deng Yinbei, Zhang Ziliang, Tang Qingwei.The Development Status of solid lithium battery.Power supply
The world, 2014,35-37.）And the disclosed solid electrolyte 20LiI- for including tetra- kinds of elements of Li, P, S, I in 2017
80Li3PS4（Patent publication No.：US 20170179545 A1）.However, the chalcogenide glass state electrolysis in above-mentioned disclosed technology
Matter easily chemically reacts in preparation process with the component in air, therefore has high requirement to working condition.And
And because the chemical reactivity between sulphion and oxonium ion is different, chalcogenide glass state electrolyte would generally be with oxygen-containing member
The anode active material of lithium ion battery of element reacts, and generates one layer of high-resistance boundary layer, reduces the performance of battery and makes
Use the life-span.Therefore, it is necessary to which the Surface coating in positive electrode active materials reacts suppression when using chalcogenide glass state electrolyte
Preparative layer（Patent publication No.：The B of CN 103534847 B, CN 103038922）, to reach stable interface and reduce interface internal resistance
Effect.
As can be seen here, develop a kind of oxide glass state electrolyte, will be expected to avoid sulphur system electrolyte and positive-active material
Between material caused by chemical reactivity difference between oxygen and sulphion interfacial reaction, and oxide glass state be electrolysed
Matter can be prepared in atmosphere, and this will greatly reduce requirement to environment in production preparation process, and this is for development low cost
High performance solid lithium battery is significant.
At present, the material system of oxide glass state electrolyte is less, it has been disclosed that technology mainly have Li2O-Al2O3-
GeO2-P2O5（Patent publication No.：WO 2013180658 A1）、Li2O-SiO2（Atsushi Sakuda, Hirokazu
Kitaura, Akitoshi Hayashi, Kiyoharu Tadanaga, and Masahiro Tatsumisago.
Modification of interface between LiCoO2 electrode and Li2S-P2S5 solid
electrolyte using Li2O-SiO2 grassy layers. Journal of The Electrochemical
Society, 2009, 156(1), A27-A32）、Li2O-B2O3-P2O5Deng.
The content of the invention
It is an object of the invention to provide a kind of Oxide electrolyte materials of new glassy state, when used in lithium battery
When in electrolyte or electrode, the Oxide electrolyte materials of described glassy state can provide higher lithium ion conductivity,
The interface resistance between electrode material and electrolyte is reduced, improves the interface stability between electrode material and electrolyte
Property.
The present invention is the following discovery based on inventor and conceived：Inorganic oxide material coats as coating layer material
In positive electrode active materials particle surface, it can play and be chemically reacted between stop electrolyte and positive electrode active materials
Effect, therefore be usually used in improve high potential positive electrode active materials interface stability.Moreover, the coating layer material can be simultaneously
Stably coexisted with positive electrode active materials and electrolyte.In addition, the coating layer material also has higher lithium ion
Conducting power.However, do not have lithium ion conduction ability when inorganic oxide material uses separately as electrolyte generally,
But but there is excellent lithium ion conduction ability during coat materials'use as positive electrode active materials, this except with its
The non-crystalline type form of surface of positive electrode active material is relevant, and shuttle process that should also be with lithium ion in layer material is coated is close
It is related.It may be shuttled just because of lithium ion in inorganic oxide coats layer material and enter positive electrode active materials or electrolyte
When, there occurs the phenomenon that appropriate lithium ion is rested in inorganic oxide coating layer material, change inorganic oxide coating
The component of layer material, and it is possessed the ability of quick conducting lithium ions.
The technical solution adopted by the present invention is to achieve the above object：
A kind of Oxide electrolyte materials of glassy state, the Oxide electrolyte materials chemical formula Li of glassy statexM1yM2y’Oz
Representing, M1 is magnesium, aluminium, titanium, iron, copper, zinc, zirconium, tin, cerium, the one or more among lanthanum, and M2 is boron, carbon, nitrogen, fluorine, silicon, phosphorus,
One or more among sulphur, x, y, y ', z span be 1<X≤10,0≤y≤5,0≤y '≤3,0<Z≤12, wherein,
When M1 is titanium and y '=0, x value is not equal to 2 or 4；When M1 is titanium elements, M2 can not take P element；As y=0, x's takes
Value is not equal to 2 or 3.
The Oxide electrolyte materials of described glassy state have ionic conductivity, ionic conductivity 10-1-10-12 S/
cm。
The Oxide electrolyte materials of described glassy state are non-crystalline type structure.
The form of the Oxide electrolyte materials of described glassy state is one kind in powder, film, bulk.
A kind of application of Oxide electrolyte materials of glassy state described above in lithium cell electrolyte, described glass
The Oxide electrolyte materials of glass state are used in the liquid electrolyte, gel electrolyte or solid electrolyte of lithium battery.
The Oxide electrolyte materials of described glassy state are individually or with other materials simultaneously used in the electrolysis of lithium battery
In matter.
A kind of application of Oxide electrolyte materials of glassy state described above in electrode of lithium cell, described glass
The Oxide electrolyte materials of state are used in the electrode of lithium battery, and described electrode includes positive pole and negative pole, described glassy state
Oxide electrolyte materials existence form in the electrodes to be dispersed in the form of granules between electrode active material particles,
The active material particle surface of electrode is coated in the form of a film, is coated in the surface of electrode slice in the form of a film or with thin
The form of film or bulk is placed between electrode slice and electrolyte.
The Oxide electrolyte materials of described glassy state can use ball milling, calcining, ald, evaporation, sputtering
Prepared etc. material synthesis method, control charge condition can also be used to carry out the electrochemical method of lithiumation and prepared.
The present invention has following remarkable advantage compared with prior art：
The oxide electrolyte for the glassy state that the present invention uses has higher compatibility with positive electrode active materials, because greatly
Partial positive electrode active materials are oxides, therefore will not be occurred using sulphur system solid-state electricity using the oxide electrolyte of glassy state
Solve interfacial reaction problem common during matter.Compared with the oxide electrolyte of crystalline state, the oxide electrolyte of glassy state is not deposited
Grain boundary resistance is high the problem of.Moreover, the oxide electrolyte of glassy state is typically chemically inert, there is higher electrification
Stability is learned, disclosure satisfy that requirement of the electrode material of high potential and high electrochemical activity to electrolyte Width funtion window.Therefore,
The oxide electrolyte of glassy state proposed by the present invention has weight in the field of lithium ion battery of high-energy-density and high security
The application prospect wanted.
Brief description of the drawings
The present invention will be further described in detail with reference to the accompanying drawings and detailed description.
Fig. 1 is the SEM photograph of the oxide electrolyte of the glassy state in the embodiment 1 that the present invention designs.
Fig. 2 is the linear scan curve of the oxide electrolyte of glassy state in the embodiment 2 that the present invention designs.
Fig. 3 is the lithium cobaltate cathode activity of the oxide electrolyte coated with glassy state in the embodiment 3 that the present invention designs
The TEM photos of material granule.
Fig. 4 is filling for the lithium cobaltate cathode for the oxide electrolyte that glassy state is coated with the embodiment 3 that the present invention designs
Discharge curve.
Embodiment
The present invention is intended to provide a kind of Oxide electrolyte materials of new glassy state, the electrolyte not only can be with
Used as electrolyte in solid state lithium battery, or as electrode material a part be used in use electrolyte or gel
In the lithium ion battery of electrolyte, the part for being also used as electrode material is used in solid state lithium battery.
Below by embodiment, the present invention is described in further detail, but does not limit the scope of the invention.
Embodiment 1
Take Li2O、Al2O3、SiO2It is 5 according to mol ratio：1：1 ratio carries out ball milling, small with 400 revs/min of rotating speed ball milling 1
When, then well mixed powder sample is dried 12 hours in 80 °C of baking ovens.The complete powder sample of drying is placed on oxygen
Change in aluminium crucible, be incubated 5 hours in 750 °C of Muffle furnace and then in 900 °C are incubated 10 minutes, then quenched
Fire processing, you can obtain the solid electrolyte Li of glassy state10Al2SiO5Powder sample, obtained powder sample is scanned
Electron microscope（SEM）, the sample topography and particle diameter measured be as shown in Figure 1.
Embodiment 2
The use of ozone is oxidant, trimethyl aluminium is silicon source, and tert-butyl group lithium alkoxide is lithium source, and high-purity N 2 is flushing gas, using original
The method of sublayer deposition prepares Li3Al2O3.Wherein, substrate is Si (111), and reactor pressure is 3 mbar, and ozone flow velocity is 200
cm3/min.The aluminum oxide of half period is deposited by ALT pulse trimethyl aluminium and ozone, then ALT pulse tert-butyl group alcohol again
Lithium and water deposited oxide lithium, the ratio of elemental lithium and aluminium element is controlled by adjusting the burst length, finally obtain the oxygen of glassy state
Compound electrolytic thin-membrane Li3Al2O3.Obtained film sample is sprayed into electrolyte the sweeping with 0.1V/s in electrochemical workstation afterwards
Speed carries out linear scan, you can the electrochemical window of the dielectric film of survey, if shown in 2, the electrification of prepared dielectric film
Learn stability window and be more than 4.5 V.
Embodiment 3
0.1 mol/L sodium bicarbonate solution and 0.1 mol/L aluminum sulfate solution are prepared respectively first, then by cobalt acid lithium powder
End is added in sodium bicarbonate solution, the min of ultrasonic disperse 20, then the aluminum sulfate solution prepared is added into solution, obtains hydroxide
The cobalt acid lithium powder of aluminium cladding.The cobalt acid lithium powder of aluminium hydroxide cladding is separated, is dried, is placed in 300 °C of Muffle furnaces and heats
2 hours, then proceed to be warming up to 600 °C and heat 6 hours, you can obtain the cobalt acid lithium powder of alumina-coated.In order to obtain
Li1.8Al2O3The cobalt acid lithium powder of cladding is, it is necessary to cobalt acid lithium powder and conductive agent by alumina-coated（Such as acetylene black）, bond
Agent（Such as PVDF）According to 8：1：Coated on titanium foil after 1 mass ratio is well mixed, electrode slice and assembled battery is made.Then
With low current（0.01C multiplying power）0.05 V is discharged to 3 times repeatedly to positive plate progress, realized to coated in cobalt acid lithium surface
Aluminum oxide lithiumation process, you can obtain the Li of non-stoichiometric1.8Al2O3The cobalt acid lithium powder of cladding.As shown in figure 3,
The Li on cobalt acid lithium surface1.8Al2O3Clad is glassy state, the nm of thickness about 200.Use Li1.8Al2O3The lithium cobaltate cathode piece of cladding
With lithium metal, 1 mol/L LiPF6Ethylene carbonate/diethyl carbonate (volume ratio 1：1) electrolyte is assembled into button electricity
Pond, discharge and recharge is carried out with 1C multiplying power in 3.0-4.6 V, can be 100 weeks with stable circulation, specific charging and discharging curve is as shown in Figure 4.
Claims (7)
- A kind of 1. Oxide electrolyte materials of glassy state, it is characterised in that the Oxide electrolyte materials chemistry of glassy state Formula LixM1yM2y’OzRepresent, wherein, M1 is magnesium, aluminium, titanium, iron, copper, zinc, zirconium, tin, cerium, the one or more among lanthanum, and M2 is Boron, carbon, nitrogen, fluorine, silicon, phosphorus, the one or more among sulphur, x, y, y ', z span be 1<X≤10,0≤y≤5,0≤ Y '≤3,0<Z≤12, wherein, when M1 is titanium and y '=0, x value is not equal to 2 or 4；When M1 is titanium elements, M2 can not take P element；As y=0, x value is not equal to 2 or 3.
- A kind of 2. Oxide electrolyte materials of glassy state according to claim 1, it is characterised in that described glassy state Oxide electrolyte materials there is ionic conductivity, ionic conductivity 10-1-10-12 S/cm。
- A kind of 3. Oxide electrolyte materials of glassy state according to claim 1, it is characterised in that described glassy state Oxide electrolyte materials be non-crystalline type structure.
- A kind of 4. Oxide electrolyte materials of glassy state according to claim 1, it is characterised in that described glassy state Oxide electrolyte materials form be powder, film, one kind in bulk.
- 5. a kind of application of Oxide electrolyte materials of glassy state according to claim 1 in lithium cell electrolyte, Characterized in that, the Oxide electrolyte materials of described glassy state be used in the liquid electrolyte of lithium battery, gel electrolyte or In solid electrolyte.
- 6. a kind of application of Oxide electrolyte materials of glassy state according to claim 5 in lithium cell electrolyte, Characterized in that, the Oxide electrolyte materials of described glassy state are individually or with other materials simultaneously used in the electricity of lithium battery Xie Zhizhong.
- 7. a kind of application of the Oxide electrolyte materials of the glassy state described in claim 1 in electrode of lithium cell, its feature It is, the Oxide electrolyte materials of described glassy state are used in the electrode of lithium battery, and described electrode includes positive pole and born Pole, the existence form of the Oxide electrolyte materials of described glassy state in the electrodes is is dispersed in electrode active in the form of granules Property material granule between, in the form of a film coated in electrode active material particle surface, in the form of a film coated in electricity The surface of pole piece is placed between electrode slice and electrolyte in the form of film or bulk.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111446494A (en) * | 2020-04-17 | 2020-07-24 | 上海空间电源研究所 | Glass state lithium ion solid electrolyte and preparation method thereof |
| CN110323489B (en) * | 2019-06-28 | 2020-09-08 | 华中科技大学 | Solid lithium ion conductor and preparation method and application thereof |
| CN111952552A (en) * | 2019-05-17 | 2020-11-17 | 湖南杉杉能源科技股份有限公司 | Glass state coated positive electrode material and preparation method thereof |
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Application publication date: 20180330 |