CN207719320U - A kind of modified lithium battery electrode structure, lithium battery structure - Google Patents
A kind of modified lithium battery electrode structure, lithium battery structure Download PDFInfo
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- CN207719320U CN207719320U CN201721785123.6U CN201721785123U CN207719320U CN 207719320 U CN207719320 U CN 207719320U CN 201721785123 U CN201721785123 U CN 201721785123U CN 207719320 U CN207719320 U CN 207719320U
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Abstract
The utility model is related to technical field of lithium batteries more particularly to a kind of modified lithium battery electrode structures and lithium battery structure.A kind of modified lithium battery electrode structure, the modified lithium battery electrode structure include Li for electrolyte7La3Zr2O12Lithium battery in, which includes electrode layer and the buffer structure layer that is formed on the electrode layer, and the buffer structure layer includes the oxide containing lithium, lanthanum, zirconium and tantalum.Buffer structure layer is formed on electrode structure layer, the buffer structure layer includes the oxide containing lithium, lanthanum, zirconium and tantalum.The fermi level of buffer structure layer is between electrode structure and electrolyte, transmission potential barrier of the lithium ion between electrolyte and electrode structure can be reduced well, the interface impedance between electrolyte and electrode structure can be reduced well, improve the conductive performance of conductive ion.
Description
【Technical field】
The utility model is related to technical field of lithium batteries more particularly to a kind of modified lithium battery electrode structures and lithium battery knot
Structure.
【Background technology】
Solid state lithium battery has the characteristics that safe, service life is long, energy density is high, is current lithium battery research neck
One of the hot spot in domain, future are expected to be used widely in the fields such as electric vehicle and intelligent grid.In solid state lithium battery, boundary
Face characteristic is to determine the key point of battery performance.
Currently, there are solid-solid interface adhesiveness is bad in solid state lithium battery, it is bonded not close, electrode layer and electrolyte layer
The potential barrier of intermediate ion transmission can cause interface impedance to increase;Meanwhile the unknown pair of the stripping and inside battery between solid-solid interface
The problem that interface stability can be caused bad is reacted, battery is in turn resulted in and shortens even damage.The prior art is main
It is solid-solid interface impedance to be reduced by high-temperature process technology, but high-temperature process can be such that elements diffusion ability enhances, chemical reaction is lived
Property increase, reduce the stabilization of solid-solid interface instead, thus cannot truly reach reduce solid-solid interface between impedance,
Influence the transmission performance of conductive ion.
【Utility model content】
To overcome the problems, such as that the solid-solid interface impedance between current solid state lithium battery electrode layer and electrolyte layer is big, this reality
Engineering is buffered based on energy band with novel, the fermi level of buffer layer is modulated by doping and ion transmits potential barrier, reduces solid-state lithium
Solid-solid interface impedance between electrolyte layer and electrode layer in battery improves a kind of modified lithium battery of conductive ion conduction velocity
Electrode structure and lithium battery structure.
In order to solve the above-mentioned technical problem, the utility model provides a technical solution:
A kind of modified lithium battery electrode structure, the modified lithium battery electrode structure include Li for electrolyte7La3Zr2O12's
In lithium battery, which includes electrode layer and is formed on the electrode layer towards electrolyte layer side
Buffer structure layer, the buffer structure layer includes the oxide containing lithium, lanthanum, zirconium and tantalum.
Preferably, the electrode layer includes anode layer and negative electrode layer.
Preferably, it is Li that the buffer structure layer, which includes the oxide containing lithium, lanthanum, zirconium and tantalum,7-xLa3Zr2-xTaxO12,
The value of the x is more than 0 and is less than 2.
Preferably, the anode layer include include plus plate current-collecting body and the monocrystalline being formed on plus plate current-collecting body anode
Film.
Preferably, the monocrystalline cathode film by MOx without oxidate for lithium monocrystalline anode Crystallization.
Preferably, the thickness of the buffer structure layer is:2-20nm.
In order to solve the above-mentioned technical problem the utility model, provides another technical solution, a kind of lithium battery structure, including such as
Modified lithium battery electrode structure described above and electrolyte layer, the electrolyte layer include Li7La3Zr2O12, the electrode knot
Structure includes anode layer and negative electrode layer, and the electrolyte is formed between the anode layer and negative electrode layer.
Compared with prior art, be formed with buffer structure layer on electrode structure, the buffer structure layer include containing lithium,
The oxide of lanthanum, zirconium and tantalum, electrolyte include Li7La3Zr2O12.The fermi level of buffer structure layer is in electrode structure and electrolysis
Between matter, transmission potential barrier of the lithium ion between electrolyte and electrode structure can be reduced well, can reduce electrolyte well
Interface impedance between electrode structure improves the conductive performance of conductive ion.
The electrode layer includes anode layer and negative electrode layer, the buffer structure layer can be formed in anode layer and negative electrode layer it
On in one or both so that buffer structure layer can be formed in corresponding electrode well according to the demand of electric conductivity
On layer, the demand for reducing interface impedance is better met.
The buffer structure layer includes that the oxide chemistry general formula containing lithium, lanthanum, zirconium and tantalum is Li7-xLa3Zr2-xTaxO12,
The value of the x is more than 0 and is less than 2.Itself and electrolyte Li7La3Zr2O12Difference lies in utilize Ta5+Instead of the electrolyte
Li7La3Zr2O12Middle part Zr4+Position.Ta is inert metal, under relatively low sintering temperature, cubic garnet knot
Structure is stablized.Work as Ta5+Instead of the Zr of part4+After position, due to Ta5+With 5 valence electrons, Li is reduced+Content, to
Improve Li+Vacancy concentration, be conducive to improve buffer structure layer Li7-xLa3Zr2-xTaxO12Middle Li+Conductivity so that buffering knot
The conductivity of structure layer improves.
The thickness of the buffer structure layer is:2-20nm can reduce the interface between electrolyte and electrode structure well
Impedance ensures conductive performance of the conductive ion between electrolyte and buffering structure sheaf.
The two of the purpose of this utility model are to provide a kind of modified lithium battery electrode structure as described above and electrolysis
Matter layer, the electrolyte layer include Li7La3Zr2O12, the electrode of lithium cell structure includes anode layer and negative electrode layer, the electricity
Matter is solved to be arranged between the anode layer and negative electrode layer.The electrolyte layer includes Li7La3Zr2O12.The buffer structure layer packet
Include Li7-xLa3Zr2-xTaxO12, the fermi level of buffer structure layer is between anode layer and electrolyte layer;Alternatively, buffer structure
The fermi level of layer is between negative electrode layer and electrolyte layer, can reduce lithium ion well between electrolyte layer and anode layer
Either the transmission potential barrier between negative electrode layer can reduce electrolyte layer and anode layer or electrolyte layer in lithium battery structure well
Interface impedance between negative electrode layer improves the conductive performance of conductive ion.
【Description of the drawings】
Fig. 1 is that buffer structure layer is formed in the modified lithium battery electrode structure formed on anode layer and shows in the utility model
It is intended to;
Fig. 2 is that buffer structure layer is formed in the modified lithium battery electrode structure formed on negative electrode layer and shows in the utility model
It is intended to;
Fig. 3 is positive schematic diagram of a layer structure in the utility model;
Fig. 4 is the preparation flow figure of buffer structure layer in the utility model;
Fig. 5 is in the utility model by the stream on the buffer structure layer target as sputter to anode layer and/or negative electrode layer
Cheng Tu;
Fig. 6 is the overall structure diagram of lithium battery structure in the utility model;
Fig. 7 is electron energy band figure in the utility model;
Fig. 8 is to be formed with the lithium battery structure of buffer structure layer and the boundary of the lithium battery structure of buffer structure layer is not formed
Face impedance variations effect contrast figure.
【Specific implementation mode】
The above is only the preferred embodiment of the utility model only, is not intended to limit the utility model, all at this
Any modification made by within the principle of utility model, equivalent replacement and improvement etc. should all include the scope of protection of the utility model
Within.
It please refers to Fig.1 and Fig. 2, a kind of modified lithium battery electrode structure 10, the modified lithium battery electrode structure 10 is used for electricity
It includes Li to solve matter7La3Zr2O12Lithium battery in, which includes electrode layer and being formed in the electrode
Buffer structure layer 30 on layer.The electrode layer includes anode layer 201 and negative electrode layer 202, and the buffer structure layer 30 can be with
It is formed in the anode layer 201 and the one of negative electrode layer 202, or is formed simultaneously on the two.The buffer structure layer
30 include the oxide containing lithium, lanthanum, zirconium and tantalum, and the buffer structure layer 30 includes that the oxide containing lithium, lanthanum, zirconium and tantalum is
Li7-xLa3Zr2-xTaxO12, the value of the x is more than 0 and is less than 2.
Referring to Fig. 3, the anode layer 201 includes a plus plate current-collecting body 2011 and is formed on plus plate current-collecting body 2011
The monocrystalline cathode film 2013 formed without the positive polar crystal of oxidate for lithium monocrystalline 2012 by MOx.
The preparation method that the two of the purpose of this utility model are to provide a kind of modified lithium battery electrode structure 10 includes such as
Lower step:
S1:The oxidation containing lithium, lanthanum, zirconium and tantalum included by the buffer structure layer 30 is prepared using high temperature solid phase synthesis
Object;
S2:The oxide containing lithium, lanthanum, zirconium and tantalum included by the buffer structure layer 30 is sputtered at using magnetron sputtering method
Buffer structure layer 30 is formed on the electrode layer.
Referring to Fig. 4, being prepared included by the buffer structure layer 30 using high temperature solid phase synthesis in above-mentioned steps S1
The chemical general formula of oxide containing lithium, lanthanum, zirconium and tantalum is Li7-xLa3Zr2-xTaxO12, synthesize and be as follows:
S11:Will the synthesis oxide raw material powder mixing containing lithium, lanthanum, zirconium and tantalum and grind, that tabletting obtains powder is pre-
Product;
S12:Powder preform is subjected to first sintering, sintering temperature is 900-1000 DEG C, sintering time 10-
14h obtains the first sinter;
S13:The Li of the first sinter gross mass 1% will be accounted for3PO4It is added to the first sinter mixing and carries out
Ball milling obtains intermediate product repeatedly;
S14:The intermediate product is carried out second to be sintered, sintering temperature is 1100-1200 DEG C, sintering time 5-
The oxide of lithium included by buffer structure layer, lanthanum, zirconium and tantalum is made in 8h.
In above-mentioned steps S11, the oxide raw material powder containing lithium is selected from LiO2、LiH、LiOH·H2O、LiN、
LiCO3In one or several kinds.
The oxide raw material of the lanthanum is selected from La (OH)3、La2O3、La(NO3)3、 LaCl3Middle one or several kinds.
The oxide raw material of the zirconium is selected from ZrO2、Zr(OH)4、ZrCl4In one or several kinds.
The oxide raw material of the tantalum is Ta2O5。
Meanwhile in above-mentioned S11 steps, by the synthesis oxide raw material powder mixing containing lithium, lanthanum, zirconium and tantalum and grind
Before mill, addition grinding aid and the synthesis oxide raw material powder mixing containing lithium, lanthanum, zirconium and tantalum.
The utility model selects PD-2 powder grinding assistant modifiers, and PD-2 powder grinding assistant modifiers are a kind of compound esters surfaces
Activating agent is mainly dissolved in water, ethyl alcohol, isopropanol and most of organic solvent.Its with excellent grinding aid, dispersion, modifying function,
Powder surface free energy and ore hardness can effectively be reduced, in powder process of lapping add use, can be improved grinding efficiency and
Segment yield.In use, according to mass fraction being 1 by the PD-2 powders grinding assistant modifier and isopropanol:After 1 ratio dissolving
Obtain the grinding aid.The additive amount of grinding aid is total in the powder preform containing lithium, lanthanum, zirconium and tantalum in the step S1
The 0.07%-0.3% of quality.It is added to after grinding aid, by the grinding aid and the oxygen containing lithium, lanthanum, zirconium and tantalum
Compound raw material powder mixing, with agate ball ball milling 22-26h.
In above-mentioned steps S11, tabletting obtains powder preform, mainly will be after grinding using isostatic cool pressing technology
The oxide raw material powder containing lithium, lanthanum, zirconium and tantalum carries out cold isostatic compaction.Isostatic cool pressing technology usually uses rubber and modeling
Material makees coating mould material, and using liquid as pressure medium, under conditions of pressure is 100-300Mpa, powder mixture is suppressed
Molding, the purpose is to be sintered for next step, the processes such as forging or hot isostatic pressing provide prefabrication.
In the step S12, the powder preform is added in the forward direction powder preform for carrying out first sintering
15% LiOHH of quality sum2O.Since the time of first sintering is longer, during high temperature sintering, it is easy to lead
The loss for causing lithium ion, adds 15% LiOHH2O is to make up the loss of lithium ion during first sintering.
In the step S13, addition accounts for the Li of the first sinter gross mass 1%3PO4Into the first sinter
Main purpose is as sintering aid, Li3PO4Fusing point be 837 DEG C, fusing point is relatively low, and have ionic conductivity
Matter.Meanwhile some oxides are easy to happen crystal transfer in sintering and with larger bulk effect, this will be such that sintering causes
Difficulty occurs for densification, and easily causes blank cracking.If at this moment suitable sintering aid can be selected to be inhibited, you can promote to burn
Knot.Such as ZrO2When sintering, a certain amount of Li is added3PO4Just belong to this principle.At 1200 DEG C or so, stable monocline
ZrO2It is transformed into the ZrO in four directions2And with about 10% volume contraction so that product stability degenerates.Introduce electricity price ratio Zr+It is low
Li+, cuboidal Zr can be formed1-xLixO2Stablize solid solution, not only product is prevented to crack in this way, but also to increase crystal hollow
Site concentration makes sintering accelerate.
In step S14, intermediate obtained in the S3 is carried out second before being sintered, first with isostatic cool pressing technology
The intermediate is pressed into high-pressure-resistant vessel, the pressure of isostatic cool pressing is 100-300Mpa, then in the high-pressure-resistant vessel
Inlet cover powder preform.Inlet in the high-pressure-resistant vessel covers pulverulent product, mainly compensates the
The loss of lithium ion during once sintered.
The general formula of the oxide containing lithium, lanthanum, zirconium and tantalum in step S14 included by buffer structure layer 30 obtained is
Li7-xLa3Zr2-xTaxO12, the value of the x is:0 < x < 2.Li7-xLa3Zr2-xTaxO12With higher lithium ion conductivity.
In the present invention, the raw material for preparing the oxide containing lithium, lanthanum, zirconium and tantalum is specially LiOHH2O、La
(OH)3、ZrO2、Ta2O5。
Please referring to will be included by the buffer structure layer 30 using magnetron sputtering method in the step S2 with 1 and Fig. 5
Li7-xLa3Zr2-xTaxO12Oxide sputters at formation buffer structure layer 30 on the electrode layer and is as follows:
S21:Buffer structure layer Li7-xLa3Zr2-xTaxO12The installation of oxide target material;
S22:The anode layer 201 and/or negative electrode layer 202 are mounted in substrate frame;
S23:Vacuum is extracted into 8.8 X 10-4Pa or less;
S24:The temperature of substrate frame is heated to 300-500 DEG C;
S25:It adjusts argon gas and the ratio of oxygen, sputtering power is sputtered.
In the step S22:The anode layer 201 and/or negative electrode layer 202 are mounted in substrate frame, in sputtering process
The slewing rate of anode layer 201 and/or negative electrode layer 202 in substrate frame is 5r/min, to ensure that 30 target of buffer structure layer is heavy
Long-pending uniformity.
The ratio of argon gas and oxygen is in the step S25:1:1, sputtering power is:160W, sputtering time 6h, obtains
The thickness of buffer structure layer 30 is 2-20nm.
It please refers to Fig.1 and Fig. 6, the three of the purpose of this utility model is to provide a kind of lithium battery structure 40, the lithium electricity
Pool structure 40 includes the electrode structure 10 provided such as above-mentioned purpose of utility model one.Further, the lithium battery structure 40 can
Further comprise electrolyte 50.Electrode structure 10 includes anode layer 201 and negative electrode layer 202, the anode layer 201 and/or described
Buffer structure layer 30 is formed in the one of negative electrode layer, the electrolyte 50 is arranged between anode layer 201 and negative electrode layer 202.
Specifically, in the present invention, the electrolyte 50 includes Li7La3Zr2O12.The buffer structure layer obtained
30 include Li7-xLa3Zr2-xTaxO12, and electrolyte Li7La3Zr2O12Difference lies in utilize Ta5+Instead of the electrolyte
Li7La3Zr2O12Middle part Zr4+Position.Ta is inert metal, under relatively low sintering temperature, cubic garnet knot
Structure is stablized.Work as Ta5+Instead of the Zr of part4+After position, due to Ta5+With 5 valence electrons, Li is reduced+Content, to
Improve Li+Vacancy concentration, be conducive to improve buffer layer target Li7-xLa3Zr2-xTaxO12Middle Li+Conductivity so that buffer layer
Target Li7-xLa3Zr2-xTaxO12Conductivity improve.
Fig. 6 and Fig. 7 are please referred to, after forming buffer structure layer 30 in side of the anode layer 201 towards electrolyte 50,
The fermi level of buffer structure layer 30 is between the fermi level of anode layer 201 and the fermi level of electrolyte 50 so that is led
Electric Li+Ion is first to transit to buffer structure layer 30 from electrolyte 50, then transits to anode layer from buffering structure sheaf 30 again
201, rather than anode layer 201 directly is transitted to from electrolyte 50, conductive Li is reduced well+Ion is passed in solid phase interface
Defeated potential barrier, efficiency of transmission of the enhancing conductive ion between electrolyte 50 and anode layer 201, improves the lithium battery structure 40
Electric conductivity.
If it can also be appreciated that the side towards electrolyte 50 on negative electrode layer 202 forms the buffer structure
Layer 30 has and forms the same effect of buffer structure layer 30 in side of the anode layer 201 towards electrolyte 50.Likewise, also
It can be formed simultaneously buffering in the side towards electrolyte 50 on side of the anode layer 201 towards electrolyte 50 and negative electrode layer 202
Structure sheaf 30.
It is interface impedance variation effect figure incorporated by reference to Fig. 6 and Fig. 8, Fig. 8.To being formed with the lithium battery knot of buffer structure layer 30
Structure 40 is carried out at the same time with the lithium battery structure that buffer structure layer 30 is not formed exchanges obstruction test (EIS), forms buffering knot
Resistance of the lithium battery structure 40 in electrolyte 50 after structure layer 30 and the resistance at 201 interface of anode layer are below and are not formed
The lithium battery structure of buffer structure layer 30, and form the anode layer 201 after buffer structure layer 30 and do not occur new interface.
Compared with prior art, be formed with buffer structure layer on electrode structure, the buffer structure layer include containing lithium,
The oxide of lanthanum, zirconium and tantalum, electrolyte include Li7La3Zr2O12.The fermi level of buffer structure layer is in electrode structure and electrolysis
Between matter, transmission potential barrier of the lithium ion between electrolyte and electrode structure can be reduced well, can reduce electrolyte well
Interface impedance between electrode structure improves the conductive performance of conductive ion.
The electrode layer includes anode layer and negative electrode layer, the buffer structure layer can be formed in anode layer and negative electrode layer it
On in one or both so that buffer structure layer can be formed in corresponding electrode well according to the demand of electric conductivity
On layer, the demand for reducing interface impedance is better met.
The buffer structure layer includes that the oxide chemistry general formula containing lithium, lanthanum, zirconium and tantalum is Li7-xLa3Zr2-xTaxO12,
The value of the x is more than 0 and is less than 2.Itself and electrolyte Li7La3Zr2O12Difference lies in utilize Ta5+Instead of the electrolyte
Li7La3Zr2O12Middle part Zr4+Position.Ta is inert metal, under relatively low sintering temperature, cubic garnet knot
Structure is stablized.Work as Ta5+Instead of the Zr of part4+After position, due to Ta5+With 5 valence electrons, Li is reduced+Content, to
Improve Li+Vacancy concentration, be conducive to improve buffer structure layer Li7-xLa3Zr2-xTaxO12Middle Li+Conductivity so that buffering knot
The conductivity of structure layer improves.
The thickness of the buffer structure layer is:2-20nm can reduce the interface between electrolyte and electrode structure well
Impedance ensures conductive performance of the conductive ion between electrolyte and buffering structure sheaf.
The two of the purpose of this utility model are to provide a kind of modified lithium battery electrode structure as described above and electrolysis
Matter layer, the electrolyte layer include Li7La3Zr2O12, the electrode of lithium cell structure includes anode layer and negative electrode layer, the electricity
Matter is solved to be arranged between the anode layer and negative electrode layer.The electrolyte layer includes Li7La3Zr2O12.The buffer structure layer packet
Include Li7-xLa3Zr2-xTaxO12, the fermi level of buffer structure layer is between anode layer and electrolyte layer;Alternatively, buffer structure
The fermi level of layer is between negative electrode layer and electrolyte layer, can reduce lithium ion well between electrolyte layer and anode layer
Either the transmission potential barrier between negative electrode layer can reduce electrolyte layer and anode layer or electrolyte layer in lithium battery structure well
Interface impedance between negative electrode layer improves the conductive performance of conductive ion.
The above is only the preferred embodiment of the utility model only, is not intended to limit the utility model, all at this
Any modification made by within the principle of utility model, equivalent replacement and improvement etc. should all include the scope of protection of the utility model
Within.
Claims (7)
1. a kind of modified lithium battery electrode structure, which includes Li for electrolyte7La3Zr2O12Lithium
In battery, it is characterised in that:The modified lithium battery electrode structure includes electrode layer and is formed on the electrode layer towards electricity
The buffer structure layer of matter layer side is solved, the buffer structure layer includes the oxide containing lithium, lanthanum, zirconium and tantalum.
2. modified lithium battery electrode structure as described in claim 1, it is characterised in that:The electrode layer includes anode layer and bears
Pole layer.
3. modified lithium battery electrode structure as described in claim 1, it is characterised in that:The buffer structure layer includes containing
Lithium, lanthanum, zirconium and tantalum oxide be Li7-xLa3Zr2-xTaxO12, the value of the x is more than 0 and is less than 2.
4. modified lithium battery electrode structure as claimed in claim 2, it is characterised in that:The anode layer includes anode collection
Fluid and the monocrystalline cathode film being formed on plus plate current-collecting body.
5. modified lithium battery electrode structure as claimed in claim 4, it is characterised in that:The monocrystalline cathode film is by MOx without lithium
Oxide monocrystal anode Crystallization.
6. the modified lithium battery electrode structure as described in any one of claim 1-5, it is characterised in that:The buffer structure layer
Thickness be:2-20nm.
7. a kind of lithium battery structure, it is characterised in that:Including modified lithium battery electrode structure as described in claim 4 and electricity
Matter layer is solved, the electrolyte layer includes Li7La3Zr2O12, the electrode structure includes anode layer and negative electrode layer, the electrolyte shape
At between the anode layer and negative electrode layer.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108365166A (en) * | 2017-12-19 | 2018-08-03 | 成都亦道科技合伙企业(有限合伙) | A kind of modified lithium battery electrode structure and preparation method thereof, lithium battery structure |
CN109768215A (en) * | 2018-12-27 | 2019-05-17 | 西安交通大学 | A kind of solid state lithium battery anode low resistance interface processing method and anode structure |
CN114300733A (en) * | 2021-12-31 | 2022-04-08 | 南方科技大学 | All-solid-state thin film lithium battery and preparation method thereof |
-
2017
- 2017-12-19 CN CN201721785123.6U patent/CN207719320U/en active Active
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108365166A (en) * | 2017-12-19 | 2018-08-03 | 成都亦道科技合伙企业(有限合伙) | A kind of modified lithium battery electrode structure and preparation method thereof, lithium battery structure |
CN109768215A (en) * | 2018-12-27 | 2019-05-17 | 西安交通大学 | A kind of solid state lithium battery anode low resistance interface processing method and anode structure |
CN114300733A (en) * | 2021-12-31 | 2022-04-08 | 南方科技大学 | All-solid-state thin film lithium battery and preparation method thereof |
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Effective date of registration: 20210209 Address after: No. 88, Yingbin Avenue, Shouan Town, Pujiang County, Chengdu, Sichuan 610000 Patentee after: Chengdu Dachao Technology Co.,Ltd. Address before: No. 1609, 16th floor, Hemei Begonia Center (Tianfu maker), No. 2039, south section of Tianfu Avenue, Tianfu New District, Chengdu, Sichuan 610213 Patentee before: CHENGDU YIDAO TECHNOLOGY PARTNERSHIP (L.P.) |