CN110190328A - Solid electrolyte material, dielectric film and preparation method thereof - Google Patents
Solid electrolyte material, dielectric film and preparation method thereof Download PDFInfo
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- CN110190328A CN110190328A CN201910437936.3A CN201910437936A CN110190328A CN 110190328 A CN110190328 A CN 110190328A CN 201910437936 A CN201910437936 A CN 201910437936A CN 110190328 A CN110190328 A CN 110190328A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
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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
- H01M10/058—Construction or manufacture
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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
- H01M2300/00—Electrolytes
- H01M2300/0085—Immobilising or gelification of 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
- H01M2300/0088—Composites
- H01M2300/0091—Composites in the form of mixtures
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a kind of solid electrolyte materials, dielectric film and preparation method thereof, it the use of stannic oxide/graphene nano pipe and polymeric matrix composite material is primary raw material, on the one hand it ensure that good electrolyte/electrode interface contacts using the flexibility of polymer material, it is environment friendly and pollution-free, it is also reacted simultaneously using oxygen-containing functional group-OH a large amount of in stannic oxide/graphene nano pipe ,-COOH ,-O- with lithium, the nonuniform deposition for avoiding lithium, inhibits the growth of Li dendrite, to avoid battery short circuit.It is easy to operate in addition, preparation method of the present invention is simple, it stability and has a safety feature, the dielectric film good film-forming property being prepared, thickness is uniform；The finished battery electrochemical window mouth width of dielectric film application preparation, structural stability is good, good cycle, and ionic conductivity is high under room temperature, meets the use demand of modern electronic product.
Description
Technical field
The present invention relates to solid electrolyte fields more particularly to solid electrolyte material, dielectric film and preparation method thereof.
Background technique
Currently, mobile electronic device, electric car and power grid energy-storage system are fast-developing in worldwide, because
Requirement of this people to performances such as lithium ion battery energy density, high rate performance and cyclical stabilities is also being continuously improved.But
The security performance of lithium ion battery, especially Prospect of EVS Powered with Batteries is but unresolved always.Recently as electricity
The rapid development of electrical automobile, the safety problem as caused by lithium-ion battery electrolytes volatilization, leakage, burning, explosion are sent out again and again
It is raw, therefore the research staff in worldwide is even thorough to improve in strongly exploration lithium ion battery of new generation
Eliminate the security risk of lithium ion battery.
Compared with traditional polymer solid electrolyte material, sulfide material is easy to produce vulcanization to air and its sensitivity
The pernicious gases such as hydrogen；Polymer electrolyte mechanical strength is low, is easily pierced through by Li dendrite；Oxide material hardness is big, still
There is a problem of that interfacial contact is bad, meanwhile, Li dendrite can be grown in oxide lattice gap, lead to battery short circuit.
Summary of the invention
Goal of the invention: in order to overcome defect existing in the prior art, the invention proposes a kind of solid electrolyte material,
Dielectric film and preparation method thereof；Preparation method is simple, easy to operate, stability and has a safety feature, under room temperature ion
Conductivity is high, meets the use demand of modern electronic product.
Technical solution: in order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is as follows:
Solid electrolyte material includes 20-50 parts of stannic oxide/graphene nano pipes, 30-75 parts of solvents, 0.5-5 in mass
Part polymeric matrix, 0.2-2.5 parts of lithium salts.
The stannic oxide/graphene nano pipe contains oxygen-containing group；Oxygen-containing group makes it have good water-soluble and biofacies
Capacitive.
Further, the oxygen-containing group is hydroxyl, carboxyl, the one of which in epoxy group.
Further, the stannic oxide/graphene nano length of tube be 5-30 μm, diameter 2-20nm；Specific surface area is greater than
250m2/g。
In some embodiments, the polymeric matrix includes polyethylene oxide PEO, polyacrylonitrile (PAN), polyvinylidene fluoride
Alkene PVDF, polymetylmethacrylate, polypropylene oxide PPO, in Vingon PVDC two or more is mixed
Close object.
In some embodiments, the solvent include acetonitrile, chloroform, methylene chloride, acetone, benzene,toluene,xylene,
At least one of N,N-dimethylformamide, cyclohexanone, hexamethylene, methanol, ethyl alcohol, ether.
In some embodiments, the lithium salts includes LiTFSI, LiClO4、LiAsF4、LiPF6、LiBF4、LiBO、
LiCH3S03、LiCF3S03One or both of mixture.
The invention also discloses the dielectric films of above-mentioned solid electrolyte material preparation, specifically by composite solid electrolyte material
Material is in nitrogen or atmosphere of inert gases, and in such a way that 40-500 μm of scraper scratches, blade coating prepares dielectric film on plate；
It scrapes the dielectric film that the coats dry 15-24h in 40-130 DEG C, the vacuum drying oven of 0MPa pressure and obtains dielectric film.
The plate wherein scratched selects one of polyfluortetraethylene plate, glass plate, stainless steel plate, silica gel plate.
Inert gas is one of helium, neon, argon gas, Krypton, xenon.
The invention also discloses the preparation methods of above-mentioned solid electrolyte material, include the following steps:
(1) in a solvent by the stannic oxide/graphene nano seal of tube, ultrasound 3-5h must aoxidize stone by the way of ultrasonic disperse
Black alkene nanotube solution；
(2) under the conditions of stirring rate is 20-400rpm/min, two or more polymeric matrix is gradually stirred
It mixes and is dissolved in the resulting stannic oxide/graphene nano pipe solution of step (1)；
(3) after polymeric matrix is completely dissolved, lithium salts is added, stirring 1.5-2h obtains composite solid under 80-100rpm/min
State electrolyte.
In order to obtain effect of preferably dissolving each other, the gradually stirring condition in step (2) is to use 90-150rpm/ for the first time
Min stirs 8-10h, stirs 5-7h using 150-400rpm/min for the second time, for the third time using 100- under vacuum conditions
150rpm/min stirs 3-4h.
The utility model has the advantages that the invention has the following advantages that using stannic oxide/graphene nano pipe and polymeric matrix composite material,
On the one hand it ensure that good electrolyte/electrode interface contacts using the flexibility of polymer material, it is environment friendly and pollution-free, while also benefit
It is reacted with oxygen-containing functional group-OH a large amount of in stannic oxide/graphene nano pipe ,-COOH ,-O- with lithium, avoids the uneven of lithium
Deposition, inhibits the growth of Li dendrite, to avoid battery short circuit.In addition, preparation method of the present invention is simple, easy to operate, stability
It can and have a safety feature, the dielectric film good film-forming property being prepared, thickness is uniform；The finished battery of dielectric film application preparation
Electrochemical window mouth width, structural stability is good, good cycle, and ionic conductivity is high under room temperature, meets modern electronic product
Use demand.
Detailed description of the invention
Fig. 1 is stannic oxide/graphene nano ror molecule structural schematic diagram；
Fig. 2 is the cyclic voltammetry curve of half obstruction battery prepared by the dielectric film of comparative example 1 and embodiment 1-3 preparation
Figure；
Fig. 3 is the schematic diagram that TEM test is carried out to stannic oxide/graphene nano pipe used in embodiment 1.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail:
Embodiment 1:
The preparation method of a kind of solid electrolyte material and dielectric film, includes the following steps:
(1) be 8nm by 35 parts of diameters, length is 30 μm, specific surface area 350m2The stannic oxide/graphene nano seal of tube of/g
In 40 parts of acetonitrile solvents, ultrasound 4h obtains stannic oxide/graphene nano pipe solution by the way of ultrasonic disperse；
(2) 2.5 parts of PEO, 0.3 part of PPO are gradually stirred and is dissolved in the resulting stannic oxide/graphene nano pipe solution of step (1)
In；Wherein stirring condition used stirs 8h using 150rpm/min stirring rate for the first time；It is stirred for the second time using 300rpm/min
Mix rate stirring 5h；For third time using under vacuum condition, 100rpm/min stirring rate stirs 3h；
(3) after two kinds of polymer matrix PEO, PPO are completely dissolved, 1.2 parts of lithium salts LiPF are added6, stir under 80rpm/min
It mixes 1.5h and obtains composite solid electrolyte material.
(4) in nitrogen atmosphere environment, in such a way that 180 μm of scrapers scratch, blade coating prepares electricity on stainless steel flat plate
Solve plasma membrane；To scrape the dielectric film coated be placed in 100 DEG C, in the vacuum drying oven of 0MPa pressure dry 19h obtain dielectric film at
Product.
Embodiment 2:
The preparation method of a kind of solid electrolyte material and dielectric film, includes the following steps:
(1) be 20nm by 40 parts of diameters, length is 15 μm, specific surface area 250m2The stannic oxide/graphene nano Guan Mi of/g
It is enclosed in 50 parts of n,N-Dimethylformamide, ultrasound 5h obtains stannic oxide/graphene nano pipe solution by the way of ultrasonic disperse；
(2) 2 parts of PVDC, 1.3 parts of PVDF are gradually stirred and is dissolved in the resulting stannic oxide/graphene nano pipe solution of step (1)
In；Wherein stirring condition used stirs 9h using 100rpm/min stirring rate for the first time；It is stirred for the second time using 200rpm/min
Mix rate stirring 6h；For third time using under vacuum condition, 100rpm/min stirring rate stirs 3.5h；
(3) after two kinds of polymer matrix PVDC, PVDF are completely dissolved, 2 parts of lithium salts LiClO are added4, under 90rpm/min
Stirring 1.5h obtains composite solid electrolyte material.
(4) in argon atmosphere environment, in such a way that 260 μm of scrapers scratch, blade coating prepares electrolysis on silica gel plate
Plasma membrane；It will scrape that the dielectric film coated is placed in 130 DEG C, drying obtains dielectric film finished product for 24 hours in the vacuum drying oven of 0MPa pressure.
Embodiment 3:
The preparation method of a kind of solid electrolyte material and dielectric film, includes the following steps:
(1) be 5nm by 50 parts of diameters, length is 20 μm, specific surface area 400m2The stannic oxide/graphene nano seal of tube of/g
In n,N-Dimethylformamide, ultrasound 3h obtains stannic oxide/graphene nano pipe solution by the way of ultrasonic disperse；
(2) 1.8 parts of PVDF, 2 parts of PEO are gradually stirred and is dissolved in the resulting stannic oxide/graphene nano pipe solution of step (1)；
Wherein stirring condition used stirs 10h using 90rpm/min stirring rate for the first time；Second using 400rpm/min stirring
Rate stirs 7h；For third time using under vacuum condition, 120rpm/min stirring rate stirs 3h；
(3) after two kinds of polymer matrix PEO, PVDF are completely dissolved, 0.7 part of lithium salts LiCH is added3S03, 2.5 parts of lithium salts
1.5h is stirred under LiTFSI, 100rpm/min obtains composite solid electrolyte material.
(4) in argon atmosphere environment, in such a way that 450 μm of scrapers scratch, blade coating prepares electrolysis on silica gel plate
Plasma membrane；It will scrape that the dielectric film coated is placed in 80 DEG C, dry 20h obtains dielectric film finished product in the vacuum drying oven of 0MPa pressure.
Comparative example 1:
Remaining preparation method is identical with embodiment 2, the difference is that and being not added with stannic oxide/graphene nano pipe, specific system
Preparation Method includes the following steps:
(1) 2 parts of PVDC, 1.3 parts of PVDF are gradually stirred and is dissolved in 50 parts of N,N-dimethylformamides of solvent；It is wherein used
Stirring condition stirs 9h using 100rpm/min stirring rate for the first time；Second using the stirring of 200rpm/min stirring rate
6h；For third time using under vacuum condition, 100rpm/min stirring rate stirs 3.5h；
(2) after two kinds of polymer matrix PVDC, PVDF are completely dissolved, 2 parts of lithium salts LiClO are added4, under 90rpm/min
Stirring 1.5h obtains composite solid electrolyte material.
(3) in argon atmosphere environment, in such a way that 260 μm of scrapers scratch, blade coating prepares electrolysis on silica gel plate
Plasma membrane；It will scrape that the dielectric film coated is placed in 130 DEG C, drying obtains dielectric film finished product for 24 hours in the vacuum drying oven of 0MPa pressure.
Prepared by the dielectric film and comparative example 1 that Example 1-3 is prepared is not added with stannic oxide/graphene nano pipe
Dielectric film is assembled into battery and carries out performance contrast test, specific as follows:
One, test index: conductivity at room temperature, electrochemical operation window
Two, test method:
(1) conductivity at room temperature takes AC impedence method to be tested: specifically that the dielectric film of preparation is round
Stainless steel substrates be assembled into (stainless steel substrates/dielectric film/stainless steel substrates) battery, handed at room temperature with electrochemical workstation
Flow impedance test；The ionic conductivity σ of dielectric film is calculated by testing obtained ac impedance spectroscopy and formula σ=t/RA.Its
In, t is the thickness of dielectric film, and R is the resistance value of dielectric film, and A is the cross-sectional area of dielectric film.
(2) electrochemical operation window takes cyclic voltammetry to be tested: specifically that the dielectric film of preparation is round
Stainless steel substrates and metal lithium sheet be assembled into (stainless steel substrates/dielectric film/metal lithium sheet) battery, carried out with electrochemical workstation
The test of electrochemical operation window, obtains linear sweep voltammetry curve.
Test result:
(1) it please refers to shown in table 1, the conductivity at room temperature of comparative example 1 is 2.2 × 10-3S·cm-1, and embodiment 1
Conductivity at room temperature is 4.6 × 10-3S·cm-1, the conductivity at room temperature of embodiment 2 is 5.1 × 10-3S·cm-1；Implement
The conductivity at room temperature of example 3 is 5.4 × 10-3S·cm-1；It can be seen that embodiment 1-3 is added to stannic oxide/graphene nano pipe
The dielectric film being prepared has higher conductivity at room temperature.
1 embodiment 1-3 of table and the comparison of 1 conductivity at room temperature of comparative example
(2) it please refers to shown in Fig. 2, is half obstruction battery prepared by the dielectric film of comparative example 1 and embodiment 1-3 preparation
Cyclic voltammetry curve figure, the upper data shown can be seen that in comparative example 1 according to fig. 2, electrochemical operation window be 0-4.5V with
It is interior, and the electrochemical operation window of embodiment 1-3 is 0-6V, it is even higher that highest can reach 6V or more；It can be seen that implementing
Example 1-3 is added to stannic oxide/graphene nano control dielectric film for made of and has higher electrochemical operation window；It can be with
The positive electrode stable matching of high voltage system, and then the higher solid state battery of energy density can be obtained.
In addition, Fig. 3 is the schematic diagram for carrying out TEM test to stannic oxide/graphene nano pipe used in embodiment 1, stone is aoxidized
Black alkene nanometer bore is 8nm.
It should be pointed out that the above specific embodiment is only illustrative of the invention and is not intended to limit the scope of the invention,
After having read the present invention, those skilled in the art fall within power appended by the application to the modification of various equivalent forms of the invention
Benefit requires limited range.
Claims (10)
1. a kind of solid electrolyte material, it is characterised in that calculated by mass includes 20-50 parts of stannic oxide/graphene nano pipes, 30-
75 parts of solvents, 0.5-5 parts of polymeric matrixs, 0.2-2.5 parts of lithium salts.
2. solid electrolyte material according to claim 1, it is characterised in that: the stannic oxide/graphene nano pipe contains
Oxygen groups.
3. solid electrolyte material according to claim 2, it is characterised in that: the oxygen-containing group is hydroxyl, carboxyl, ring
One of oxygroup.
4. solid electrolyte material according to claim 1, it is characterised in that: the stannic oxide/graphene nano length of tube is
5-30 μm, diameter 2-20nm；Specific surface area is greater than 250m2/g。
5. solid electrolyte material according to claim 1, it is characterised in that: the polymeric matrix includes polycyclic oxygen second
Alkane PEO, polyacrylonitrile (PAN), Kynoar PVDF, polymetylmethacrylate, polypropylene oxide PPO, gather inclined chloroethene
Two or more mixture in alkene PVDC.
6. solid electrolyte material according to claim 1, it is characterised in that: the solvent includes acetonitrile, chloroform, dichloro
Methane, acetone, benzene,toluene,xylene, N,N-dimethylformamide, cyclohexanone, hexamethylene, methanol, ethyl alcohol, in ether extremely
Few one kind.
7. solid electrolyte material according to claim 1, it is characterised in that: the lithium salts includes LiTFSI, LiClO4、
LiAsF4、LiPF6、LiBF4、LiBO、LiCH3S03、LiCF3S03One or both of mixture.
8. a kind of dielectric film of solid electrolyte material preparation described in claim 1, it is characterised in that by solid electrolyte
Material is in nitrogen or atmosphere of inert gases, and in such a way that 40-500 μm of scraper scratches, blade coating prepares electrolyte on plate
Film；It scrapes the dielectric film that the coats dry 15-24h in 40-130 DEG C, the vacuum drying oven of 0MPa pressure and obtains dielectric film.
9. a kind of preparation method of solid electrolyte material described in claim 1, it is characterised in that include the following steps:
(1) in a solvent by the stannic oxide/graphene nano seal of tube, ultrasound 3-5h obtains graphene oxide by the way of ultrasonic disperse
Nanotube solution；
(2) under the conditions of stirring rate is 20-400rpm/min, two or more polymeric matrix is gradually stirred molten
In the resulting stannic oxide/graphene nano pipe solution of step (1)；
(3) after polymeric matrix is completely dissolved, lithium salts is added, stirring 1.5-2h obtains composite solid electricity under 80-100rpm/min
Solve material.
10. the preparation method of solid electrolyte material according to claim 9, it is characterised in that in step (2) gradually
Stirring condition is to stir 8-10h using 90-150rpm/min for the first time, stirs 5-7h using 150-400rpm/min for the second time,
Third time stirs 3-4h using 100-150rpm/min under vacuum conditions.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110592807A (en) * | 2019-09-18 | 2019-12-20 | 宁波大学 | Thin film material for inhibiting growth of lithium dendrite and preparation method thereof |
| CN114614077A (en) * | 2022-02-24 | 2022-06-10 | 广西科技大学 | Preparation method and application of graphene composite polymer solid electrolyte membrane |
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Application publication date: 20190830 |