CN110380133A - A kind of transition zone design method of inorganic solid electrolyte and positive interpolar - Google Patents
A kind of transition zone design method of inorganic solid electrolyte and positive interpolar Download PDFInfo
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Abstract
The invention discloses the transition zone design methods of a kind of inorganic solid electrolyte and positive interpolar, belong to all-solid-state battery technical field, the design method includes: positive electrode active materials and inorganic electrolyte material to be carried out ball milling mixing by setting ratio first, and be configured to the transition zone slurry of different proportion；Then the transition zone slurry of these different proportions is coated on positive electrode surface by gradient sequence；The positive plate and inorganic solid electrolyte piece for being finally coated with gradient transitional lay fit closely together, and gradient transitional lay is between positive plate and inorganic solid electrolyte.The present invention is by introducing gradient transitional lay between anode and inorganic electrolyte, reduce between anode and inorganic electrolyte because of the problems such as gap caused by particle microscopic dimensions and microstructural differences and crystal boundary, and the transmission for existing for lithium ion of gradient transitional lay provides effective access, the interface transport resistance that further reduced ion, improves the cyclical stability of all-solid-state battery.
Description
Technical field
The invention belongs to all-solid-state battery technical fields, and it is compatible with positive interface to be related to a kind of raising inorganic solid electrolyte
A kind of design method of property, and in particular to transition zone design method of inorganic solid electrolyte and positive interpolar.
Background technique
In recent years, with the development of portable consumer electronics product and electric car, the high, cyclical stability to energy density
Good, operating voltage height, the demand for the lithium ion battery (LIBs) that can be quickly charged and discharged are increasing.However, traditional lithium ion
Battery is using liquid electrolyte, wherein existing in cell operation and letting out containing a large amount of inflammable and explosive organic solvents
The security risk of leakage, burning, explosion, while conventional membrane is easily punctured by Li dendrite, so that it is big to cause internal short-circuit of battery to generate
Calorimetric amount causes the generation of catastrophic failure.
Solid electrolyte there is non-combustible, corrosion-free, thermal and electrochemical to stablize good etc. excellent due to being free of any organic liquid
Point, while its high modulus of shearing can effectively inhibit the growth of Li dendrite.Therefore, organic liquid is replaced using solid electrolyte
Electrolyte can fundamentally solve the safety issue of traditional lithium battery, also make high-energy density cathode of lithium and high-voltage positive electrode
Using being possibly realized.Currently, solid electrolyte is roughly divided into three categories: solid polyelectrolyte, inorganic solid electrolyte and
Composite solid electrolyte.Wherein, the low problem of both rear generally existing room-temperature conductivity, and effective solution is not found yet
Scheme.Inorganic solid electrolyte is with its high lithium ion transference number, high ionic conductivity, excellent electrochemistry and thermal stability
And the extensive concern by researchers.However due between inorganic solid electrolyte and positive electrode be solid-solid contact, and
The difference of microscopic dimensions and microstructure causes its interface problem prominent, influences lithium ion in the transmission at interface.
Summary of the invention
For the interface problem of inorganic solid electrolyte in the prior art and positive interpolar, the purpose of the present invention is to provide one
The transition zone design method of kind inorganic solid electrolyte and positive interpolar, to reduce lithium ion in inorganic electrolyte and positive interpolar
Transport resistance.
In order to achieve the above technical purposes, the present invention provides a kind of inorganic solid electrolyte and the transition zone of positive interpolar designs
Method, comprising the following steps:
S1, positive electrode active materials and inorganic electrolyte material are mixed by setting ratio, after ball-milling treatment, obtains one
The transition zone powder body material of serial different proportion；
S2, the transition zone powder body material of different proportion, conductive agent, binder and dispersing agent are ground, is uniformly mixed, obtains
A series of transition zone slurry of different proportions；
S3, the transition zone slurry of different proportion is subjected to gradient sequence according to positive electrode content from high to low, is successively applied
It is overlying on positive electrode surface, through drying, roll-in, is cut, the positive plate of coating gradient transitional lay is obtained；
S4, the positive plate for coating gradient transitional lay and inorganic solid electrolyte piece are fitted closely together, and is handled well
Negative electrode tab be assembled into all-solid-state battery together.
Preferred scheme, positive electrode active materials described in step S1 are LiFePO4 (LiFePO4), nickle cobalt lithium manganate
(LiNi1-x-yCoxMnyO2), nickel cobalt lithium aluminate (LiNi1-x-yCoxAlyO2), cobalt acid lithium (LiCoO2), LiMn2O4 (LiMnO2、
LiMn2O4), nickel ion doped (LiNi0.5Mn1.5O4), one or more of organic sulfur compound material and sulphur-carbon composite.
Preferred scheme, the time of ball-milling treatment described in step S1 are 4~12h.
Preferred scheme, inorganic electrolyte material described in step S1 be NASICON type, Ca-Ti ore type, anti-perovskite type,
One or more of Garnet type oxide solid electrolyte and crystalline state, glass ceramics sulfide solid electrolyte.
Preferred scheme, the mass percent of positive electrode active materials is 30wt% in transition zone powder body material described in step S1
~70wt%, the mass percent of inorganic electrolyte material powder are 70wt%~30wt%.
Preferred scheme, conductive agent described in step S2 are Super P, acetylene black, electrically conductive graphite, carbon nanotube, graphene
One or more of.
Preferred scheme, binder described in step S2 is polyvinylidene fluoride (PVDF), polyethylene oxide (PEO), poly- inclined
One or more of difluoroethylene-hexafluoropropene (PVDF-HFP).
Preferred scheme, dispersing agent described in step S2 is N-Methyl pyrrolidone (NMP), acetonitrile (ACN), methanol, ethyl alcohol,
One or more of dimethylformamide (DMF), tetrahydrofuran (THF).
Preferred scheme, the mass percent of transition zone slurry each component described in step S2 are as follows: transition zone powder body material
45wt%~90wt%；Conductive agent 1wt%~20wt%；Binder 3wt%~15wt%；Dispersing agent 5wt%~35wt%, respectively
The sum of constituent mass percentage is 100%.
Preferred scheme, in gradient transitional lay described in step S3, each ladder layer with a thickness of 2~20 μm.
Preferred scheme, gradient transitional lay described in step S3 include 2~6 terraced layers.
Advantageous effects of the invention are as follows:
(1) present invention reduces anode and inorganic electrolyte by introducing gradient transitional lay between anode and inorganic electrolyte
Between matter because of the problems such as gap caused by particle microscopic dimensions and microstructural differences and crystal boundary, and gradient transitional lay exists for
The transmission of lithium ion provides effective access, not only effectively reduces the interface transport resistance of ion, but also improves complete solid
The cyclical stability of state battery.
(2) present invention carries out gradient coating on positive plate surface by preparing the transition zone slurry of different proportion, so that terraced
Thickness degree, coating the number of plies facilitate it is controllable, convenient for large-scale production operation.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the present invention for having the gradient transitional lay of inorganic solid electrolyte and anode.
A- plus plate current-collecting body；B- positive electrode active materials；C- cathode buffer layer；D- inorganic electrolyte；E- cathode buffer layer；f-
Lithium piece cathode.
Fig. 2 be the embodiment of the present invention 1, comparative example 1-1, comparative example 1-2 preparation all-solid-state battery impedance contrast figure.
Specific embodiment
In embodiments of the present invention, unless otherwise instructed, the means of use are the means of this field routine, the examination of use
Agent can be obtained by conventional commercial sources.
In order to clearly explain the invention, it is illustrated below by specific embodiment and attached drawing, needs to state
It is that the present invention is not limited to the specific embodiments in this specification.
Embodiment 1
By lithium iron phosphate positive material powder and LATP solid electrolyte powder 6.5:3.5,5:5 and 3.5 in mass ratio:
6.5 mixing, respectively with 500 revs/min revolution ball milling 5.5h, 7h and 8.5h.In 80 DEG C of vacuum drying 12h, three are successively obtained
The transition zone powder body material that kind arranges in gradient.By transition zone powder body material, Super P conductive agent, PVDF binder and NMP points
Powder is mixed in a certain ratio uniformly, and three kinds of transition zone slurries of arrangement of gradients are made.From high to low according to LiFePO4 content
Gradient sequence, successively be coated on iron phosphate lithium positive pole surface, every layer of coat thickness is about 6 μm.Diameter 12mm is used after roll-in
Circular die cut, and in 80 DEG C of vacuum drying 12h, obtain the positive plate of coating gradient transitional lay.
The positive plate for coating gradient transitional lay and LATP solid electrolyte piece are fitted closely together, glove box is transferred into
(water content < 1ppm, oxygen content < 1ppm), is assembled into together with the cathode lithium piece of surface modification PEO gel electrolyte film
LIR2032 steel shell button cell.
Comparative example 1-1
Difference from example 1 is that the inorganic solid electrolyte and positive interpolar in comparative example 1-1 do not have transition zone.
Comparative example 1-2
Difference from example 1 is that the inorganic solid electrolyte and positive interpolar in comparative example 1-2 are equipped with single layer mistake
Cross layer, transition zone using lithium iron phosphate positive material powder and LATP solid electrolyte powder 6.5:3.5 in mass ratio preparation and
At thickness is about 18 μm.
Embodiment 2
By nickel-cobalt lithium manganate cathode material powder and LATP solid electrolyte powder 7:3,6:4,5:5,4:6 in mass ratio and
3:7 mixing, respectively with 500 revs/min revolution ball milling 5h, 6h, 7h, 8h and 9h.In 80 DEG C of vacuum drying 12h, successively obtain
Five kinds of transition zone powder body materials arranged in gradient.By transition zone powder body material, Super P conductive agent, PEO binder and acetonitrile
Dispersing agent is mixed in a certain ratio uniformly, and five kinds of transition zone slurries of arrangement of gradients are made.According to nickle cobalt lithium manganate content by height
To low gradient sequence, it is successively coated on nickle cobalt lithium manganate positive electrode surface, every layer of coat thickness is about 5 μm.With straight after roll-in
The circular die of diameter 12mm is cut, and in 80 DEG C of vacuum drying 12h, obtains the positive plate of coating gradient transitional lay.
The positive plate for coating gradient transitional lay and LATP solid electrolyte piece are fitted closely together, glove box is transferred into
(water content < 1ppm, oxygen content < 1ppm), is assembled into together with the cathode lithium piece of surface modification PEO gel electrolyte film
LIR2032 steel shell button cell.
Comparative example 2-1
With embodiment 2 the difference is that inorganic solid electrolyte and positive interpolar in comparative example 2-1 do not have transition zone.
Comparative example 2-2
With embodiment 2 the difference is that inorganic solid electrolyte and positive interpolar in comparative example 2-2 are equipped with single layer mistake
Layer is crossed, transition zone is prepared using nickel-cobalt lithium manganate cathode material powder and LATP solid electrolyte powder 6.5:3.5 in mass ratio
It forms, thickness is about 18 μm.
Embodiment 3
By nickel cobalt lithium aluminate cathode material powder and LLZO solid electrolyte powder 6.5:3.5,5.5:4.5 in mass ratio,
4.5:5.5 and 3.5:6.5 mixing, respectively with 500 revs/min revolution ball milling 5.5h, 7h, 8.5h and 10h.It is dry in 80 DEG C of vacuum
Dry 12h successively obtains four kinds of transition zone powder body materials arranged in gradient.By transition zone powder body material, Super P conductive agent,
PVDF binder and NMP dispersing agent are mixed in a certain ratio uniformly, and four kinds of transition zone slurries of arrangement of gradients are made.According to nickel cobalt
The gradient sequence of aluminic acid lithium content from high to low is successively coated on nickel cobalt lithium aluminate positive electrode surface, and every layer of coat thickness is about 6
μm.It is cut after roll-in with the circular die of diameter 12mm, and in 80 DEG C of vacuum drying 12h, is obtaining coating gradient transitional lay just
Pole piece.
The positive plate for coating gradient transitional lay and LLZO solid electrolyte piece are fitted closely together, glove box is transferred into
(water content < 1ppm, oxygen content < 1ppm), is assembled into together with the cathode lithium piece of surface modification PEO gel electrolyte film
LIR2032 steel shell button cell.
Comparative example 3-1
With embodiment 3 the difference is that inorganic solid electrolyte and positive interpolar in comparative example 3-1 do not have transition zone.
Comparative example 3-2
With embodiment 3 the difference is that inorganic solid electrolyte and positive interpolar in comparative example 3-2 are equipped with single layer mistake
Layer is crossed, transition zone is prepared using nickel cobalt lithium aluminate cathode material powder and LLZO solid electrolyte powder 6.5:3.5 in mass ratio
It forms, thickness is about 18 μm.
Embodiment 4
By spinel nickel manganate cathode material for lithium powder and LLTO solid electrolyte powder 6.5:3.5 in mass ratio, 5.5:
4.5,4.5:5.5 and 3.5:6.5 mixing, respectively with 500 revs/min revolution ball milling 5.5h, 7h, 8.5h and 10h.It is true at 80 DEG C
The dry 12h of sky, successively obtains four kinds of transition zone powder body materials arranged in gradient.Transition zone powder body material, Super P is conductive
Agent, PVDF binder and NMP dispersing agent are mixed in a certain ratio uniformly, and four kinds of transition zone slurries of arrangement of gradients are made.According to
The gradient sequence of nickel ion doped content from high to low is successively coated on nickel ion doped positive electrode surface, and every layer of coat thickness is about 6
μm.It is cut after roll-in with the circular die of diameter 12mm, and in 80 DEG C of vacuum drying 12h, is obtaining coating gradient transitional lay just
Pole piece.
The positive plate for coating gradient transitional lay and LLTO solid electrolyte piece are fitted closely together, glove box is transferred into
(water content < 1ppm, oxygen content < 1ppm), is assembled into together with the cathode lithium piece of surface modification PEO gel electrolyte film
LIR2032 steel shell button cell.
Comparative example 4-1
With embodiment 4 the difference is that inorganic solid electrolyte and positive interpolar in comparative example 4-1 do not have transition zone.
Comparative example 4-2
With embodiment 4 the difference is that inorganic solid electrolyte and positive interpolar in comparative example 4-2 are equipped with single layer mistake
Layer is crossed, transition zone uses spinel nickel manganate cathode material for lithium powder and LLTO solid electrolyte powder 6.5:3.5 in mass ratio
It is prepared, thickness is about 18 μm.
The all-solid-state battery assembled to above-described embodiment and comparative example carries out ac impedance measurement, the interface impedance measured
Data are as shown in table 1, and as can be seen from the table, the introducing of inorganic solid electrolyte and positive interpolar gradient transitional lay can be bright
The aobvious interface impedance for reducing battery.By taking embodiment 1, comparative example 1-1, comparative example 1-2 as an example, Fig. 2 illustrates its ac impedance spectroscopy
Comparison diagram has single layer transition figure it is seen that the all-solid-state battery interface impedance without gradient transitional lay modification is 10928 Ω
The interface impedance of the all-solid-state battery of layer modification is 1511 Ω, and the all-solid-state battery interface impedance for having gradient transitional lay to modify is
75.1Ω.It can be seen that introducing single layer buffer layer material between anode and inorganic solid electrolyte can reduce to a certain extent
Its interface impedance, but interface impedance is still larger, and after introducing gradient transitional lay, interface impedance has the reduction of high degree.This
Be because be direct solid-solid contact in comparative example 1-1, between inorganic solid electrolyte and positive electrode, due to the two
Difference in terms of grain microscopic dimensions, microstructure and lithium ion transport mechanism, causes interface impedance very big.In comparative example 1-
In 2, single layer transition zone is introduced between inorganic solid electrolyte and positive electrode, so that having positive electrode-positive electrode in interface
Or the effective contact of inorganic solid electrolyte-inorganic solid electrolyte, effective transmission channel is provided to lithium ion, to a certain degree
Ground reduces interface impedance.In the embodiment of the present invention 1, the mistake that anode/inorganic solid electrolyte material arranges in gradient is introduced
Layer is crossed, the overwhelming majority is accounted in the side inorganic solid electrolyte material close to inorganic solid electrolyte, close to positive electrode
Side positive electrode accounts for exhausted most regions, and the transition of gradient substantially increases effective access of lithium ion transport, reduce because
Interface transport resistance caused by particle microscopic dimensions and microstructural differences.
The all-solid-state battery that 1 embodiment and comparative example of table is assembled carries out ac impedance measurement result
The above content is only specific implementation case of the invention, and all application cases of non-present invention, all by the present invention
Technical idea and the scheme changed is done in technical thought of the invention, the protection scope of claims of the present invention it
It is interior.
Claims (10)
1. the transition zone design method of a kind of inorganic solid electrolyte and positive interpolar, which comprises the following steps:
S1, positive electrode active materials and inorganic electrolyte material are mixed by setting ratio, after ball-milling treatment, is obtained a series of
The transition zone powder body material of different proportion；
S2, the transition zone powder body material of different proportion, conductive agent, binder and dispersing agent are ground, is uniformly mixed, obtains a system
The transition zone slurry of column different proportion；
S3, the transition zone slurry of different proportion is subjected to gradient sequence according to positive electrode content from high to low, is successively coated on
Positive electrode surface through drying, roll-in, is cut, and obtains the positive plate of coating gradient transitional lay；
S4, the positive plate for coating gradient transitional lay and inorganic solid electrolyte piece are fitted closely together, it is negative with handling well
Pole piece is assembled into all-solid-state battery together.
2. the transition zone design method of inorganic solid electrolyte and positive interpolar according to claim 1, which is characterized in that step
Positive electrode active materials described in S1 are LiFePO4, nickle cobalt lithium manganate, nickel cobalt lithium aluminate, cobalt acid lithium, LiMn2O4, nickel ion doped, have
One or more of machine sulfide material and sulphur-carbon composite.
3. the transition zone design method of inorganic solid electrolyte and positive interpolar according to claim 1, which is characterized in that step
Inorganic electrolyte material described in S1 be NASICON type, Ca-Ti ore type, anti-perovskite type, Garnet type oxide solid electrolyte,
And one or more of crystalline state, glass ceramics sulfide solid electrolyte.
4. the transition zone design method of inorganic solid electrolyte and positive interpolar according to claim 1, which is characterized in that step
The mass percent of positive electrode active materials is 30wt%~70wt%, inorganic electrolyte material in transition zone powder body material described in S1
Mass percent be 70wt%~30wt%.
5. the transition zone design method of inorganic solid electrolyte and positive interpolar according to claim 1, which is characterized in that step
Conductive agent described in S2 is one or more of Super P, acetylene black, electrically conductive graphite, carbon nanotube, graphene.
6. the transition zone design method of inorganic solid electrolyte and positive interpolar according to claim 1, which is characterized in that step
Binder described in S2 is one or more of polyvinylidene fluoride, polyethylene oxide, polyvinylidene fluoride-hexafluoropropene.
7. the transition zone design method of inorganic solid electrolyte and positive interpolar according to claim 1, which is characterized in that step
Dispersing agent described in S2 is one of N-Methyl pyrrolidone, acetonitrile, methanol, ethyl alcohol, dimethylformamide, tetrahydrofuran or several
Kind.
8. the transition zone design method of inorganic solid electrolyte and positive interpolar according to claim 1, which is characterized in that step
The mass percent of transition zone slurry each component described in S2 are as follows: transition zone powder body material 45wt%~90wt%；Conductive agent 1wt%
~20wt%；Binder 3wt%~15wt%；Dispersing agent 5wt%~35wt%, the sum of each component mass percent are 100%.
9. the transition zone design method of inorganic solid electrolyte and positive interpolar according to claim 1, which is characterized in that step
In gradient transitional lay described in S3, it is each ladder layer with a thickness of 2~20 μm.
10. the transition zone design method of inorganic solid electrolyte and positive interpolar according to claim 1, which is characterized in that step
Gradient transitional lay described in rapid S3 includes 2~6 terraced layers.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111092261A (en) * | 2019-12-12 | 2020-05-01 | 中国第一汽车股份有限公司 | Solid-state battery electrode unit |
| CN111106392A (en) * | 2019-12-30 | 2020-05-05 | 华南师范大学 | Preparation method of all-solid-state electrolyte battery |
| CN112151856A (en) * | 2020-11-02 | 2020-12-29 | 武汉理工大学 | Organic/inorganic composite solid electrolyte with gradient interface structure and all-solid-state lithium battery |
| CN112186262A (en) * | 2020-10-09 | 2021-01-05 | 西安交通大学 | MLCC structure-based all-solid-state lithium ion battery and preparation method thereof |
| CN112909329A (en) * | 2019-12-04 | 2021-06-04 | 中国科学院宁波材料技术与工程研究所 | Electrode-supported ultrathin sulfide electrolyte layer and preparation method and application thereof |
| CN113488644A (en) * | 2021-06-25 | 2021-10-08 | 万向一二三股份公司 | Preparation method of high-nickel ternary material and application of high-nickel ternary material in solid-state lithium ion battery positive plate |
| CN114530574A (en) * | 2022-01-25 | 2022-05-24 | 复旦大学 | Structured all-solid-state battery composite positive electrode, preparation method thereof and all-solid-state battery |
| CN114628775A (en) * | 2021-07-08 | 2022-06-14 | 万向一二三股份公司 | LATP composite positive plate with low interface internal resistance, preparation method and all-solid-state lithium ion battery |
| CN115360320A (en) * | 2022-10-19 | 2022-11-18 | 中国科学院精密测量科学与技术创新研究院 | All-solid-state battery with low interface resistance and high lithium metal stability and preparation method thereof |
| CN115663178A (en) * | 2022-11-01 | 2023-01-31 | 湖北亿纬动力有限公司 | Cathode material with gradient structure and preparation method and application thereof |
| CN116053401A (en) * | 2022-12-30 | 2023-05-02 | 重庆太蓝新能源有限公司 | Composite positive electrode plate, preparation method thereof and lithium battery |
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| CN115663178A (en) * | 2022-11-01 | 2023-01-31 | 湖北亿纬动力有限公司 | Cathode material with gradient structure and preparation method and application thereof |
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