CN109411809A - A kind of preparation method of low temperature flexibility solid polyelectrolyte film and its application in low-temperature solid lithium ion battery - Google Patents
A kind of preparation method of low temperature flexibility solid polyelectrolyte film and its application in low-temperature solid lithium ion battery Download PDFInfo
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- 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
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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Abstract
The invention discloses a kind of preparation method of low temperature flexibility solid polyelectrolyte film and its applications in low-temperature solid lithium ion battery, belong to solid Li-ion battery technical field.Technical solution of the present invention main points are as follows: be added after mixing the plasticizer of the lithium salts of polymer quality 5% ~ 20% and polymer quality 10% ~ 50% in solvent and sufficiently dissolve, it will be added in above-mentioned solution after the inorganic particle of polymer quality 10% ~ 90% and solvent mixing and ball milling again, acquired solution is coated on carrier by blade coating or curtain coating, up to the low temperature flexibility solid polyelectrolyte film with a thickness of 20 ~ 100 μm after 60 ~ 120 DEG C of drying.The invention also discloses the application of the low temperature flexibility solid polyelectrolyte film in low-temperature solid lithium ion battery.Polymer solid electrolyte film used in low temperature solid-state lithium ion battery prepared by the present invention has good conductivity and flexibility at low temperature so that prepare under low temperature can efficiently, the solid lithium ion battery stablizing, recycle safely is possibly realized.
Description
Technical field
The invention belongs to solid Li-ion battery technical fields, and in particular to a kind of low temperature flexibility solid polyelectrolyte
The preparation method of film and its application in low-temperature solid lithium ion battery.
Background technique
With the development and progress of society, the demands such as electric car and power grid energy storage are more more and more urgent, and exploitation uses temperature
The battery wide, safety is good, energy density and power are high becomes inexorable trend.In various commercialized secondary charge and discharge devices
In, most potential is lithium ion battery.Current commercialized lithium ion battery mainly based on liquid electrolyte, mainly at
Subpackage contains LiPF6, lithium salts such as LiFSI and with cyclic carbonate (EC, PC), linear carbonate (DEC, DMC, EDC), carboxylic acid esters
Organic solvent based on (MF, MA, EA, MP etc.).Liquid electrolyte conductivity at room temperature with higher, can efficiently soak
Moisten electrode particle, therefore such battery has the low internal resistance of cell and preferable cyclical stability and forthright again near room temperature
Energy.But liquid can occur at low temperature and convert admittedly for this kind of organic electrolyte, and conductivity is caused sharply to decline, when low temperature (- 20 DEG C with
Under) internal resistance of cell can significantly increase, it is unable to satisfy cryogenic applications requirement.In addition, commonly using the electrification of organic electrolyte system at present
It learns window and is generally less than 4.5V, influence the application of high-voltage anode material, limit the raising of battery energy density.
In solid-state but substance that Ion transfer can occur as liquid is known as solid electrolyte, since which employs solid
State structure, therefore replace traditional liquid electrolyte that can efficiently solve the above problem using solid electrolyte.In solid-state electricity
Xie Zhizhong, and it is divided into inorganic solid electrolyte and organic solid-state electrolyte.Both compare, organic polyelectrolyte has preferably
Elasticity, flexibility can reduce contact resistance admittedly, be more favorable to process, but its voltage window is narrow；Inorganic particle usually has
Still poor in processability, contact impedance are big for wider electrochemical window.The compound method of the two, which is usually taken, can be improved solid-state electricity
Solve the electrical property of matter.But problems are still faced in practical application production, including polymer solid under low temperature
The problem of electrolytic conductivity is relatively low and bad mechanical property.
Therefore, find one kind still can keep the solid electrolyte membrane of high degree of flexibility to necessitate at low temperature.Make
Solid lithium ion battery of good performance is assembled with the dielectric film with high conductance and stronger mechanical performance under low temperature
This scheme also provides new power for the application of solid state battery.
Summary of the invention
The main object of the present invention is to solve the problems such as current solid electrolyte membrane low-temperature conductivity is low and flexible poor, is provided
A kind of preparation method of low temperature flexibility solid polyelectrolyte film and its application in low temperature solid-state lithium ion battery.
The present invention adopts the following technical scheme that achieve the above object, a kind of low temperature flexibility solid polyelectrolyte film
Preparation method, it is characterised in that detailed process are as follows: by the increasing of the lithium salts of polymer quality 5% ~ 20% and polymer quality 10% ~ 50%
It is added in solvent after modeling agent mixing and sufficiently dissolves, then by the inorganic particle of polymer quality 10% ~ 90% and solvent mixing and ball milling
After be added in above-mentioned solution, acquired solution is coated on carrier by blade coating or curtain coating, up to thick after 60 ~ 120 DEG C of drying
The low temperature flexibility solid polyelectrolyte film that degree is 20 ~ 100 μm；
The polymer is modified polyvinyl chloride TPE or modified polyvinyl chloride TPE and polyvinylchloride, polyvinyl fluoride PVF, gathers
Vinyl chloride PVC, nitrile rubber NBR, modified polyvinyl chloride TPE, natural rubber NB or Kynoar-hexafluoropropene PVDF-HFP
One of or a variety of mixtures；
The lithium salts is LiN (SO2CF3)2(LiTFSI), LiN (SO2F)2(LiFSI), LiB (C2O4)2(LiBOB), LiBC2O4F2
(LiDFOB) or LiClO4One of or it is a variety of；
The plasticizer is succinonitrile (SN), diethyl phthalate (DEP), ethylene carbonate (EC), propene carbonate
(PC), one of polyethylene glycol dimethyl ether (PEGDME) or kaolin or a variety of；
The solvent is N-Methyl pyrrolidone (NMP), acetonitrile, acetone, ethyl acetate, N,N-dimethylformamide (DMF), four
One of hydrogen furans (THF) or dimethyl acetamide (DMAC) are a variety of；
The inorganic particle is LLZO, Al2O3, one of LAGP or LATP or a variety of；
The carrier is one of aluminium foil, copper foil, silicone oil paper or glaxin release paper.
Further preferably, the polymer is preferably modified polyvinyl chloride TPE, modified polyvinyl chloride TPE and lithium salts
For mass ratio in 10:1 ~ 3, gained low temperature flexibility solid polyelectrolyte film has preferable cryogenic property, and the low temperature flexibility is poly-
The density for closing object solid electrolyte membrane is the half of polychloroethylene film, tensile strength and tearing strength be respectively 20-25MPa and
50-60KN/m, brittle point is -65 DEG C ~ -75 DEG C, and polychloroethylene film is only gained low temperature flexibility polymer at -40 DEG C, -15 DEG C
The order of magnitude of solid electrolyte membrane conductivity reaches 10-4S/cm。
The preparation method of low temperature flexibility solid polyelectrolyte film of the present invention, it is characterised in that specific steps
Are as follows:
Step S1: taking modified polyvinyl chloride TPE 2g and lithium salts LiTFSI 1g to be dissolved in solvents tetrahydrofurane and is stirred
It is even to obtain clarification viscous solution；
Step S2: plasticizer phthalic acid diethylester DEP 1g is added in the viscous solution obtained to step S1, is sufficiently stirred
It is uniformly mixed and obtains solution A；
Step S3: by inorganic particle LLZO 1.2g and tetrahydrofuran mixing and ball milling, mixed system B is obtained after fully dispersed；
Step S4: the mixed system B that step S3 is obtained is added in the solution A that step S2 is obtained, after being sufficiently mixed uniformly
To dispersion C；
Step S5: the dispersion C that step S4 is obtained is prolonged into stream film forming in silicone oil paper, is put into vacuum drying oven after natural drying
In 60 DEG C of dry 12h, then the isolated low temperature flexibility solid polyelectrolyte film from silicone oil paper.
Application of the low temperature flexibility solid polyelectrolyte film of the present invention in low-temperature solid lithium ion battery,
It is characterized in that detailed process are as follows: be attached at after cutting the size of the low temperature flexibility solid polyelectrolyte film as required
On positive plate, then negative electrode tab lithium piece is covered, then assembled up to low-temperature solid lithium ion battery.
Further preferably, the specific preparation process of the positive plate are as follows: by positive electrode, conductive agent, lithium salts and binder
70 ~ 90:1 in mass ratio ~ 5:4 ~ 10:5 ~ 15 is added in solvent after mixing, and anode sizing agent is obtained after fully dispersed, by anode sizing agent
It is toasted in 100 ~ 120 DEG C after being coated on the aluminium foil with a thickness of 10 ~ 20 μm up to for assembling low temperature solid-state lithium ion battery just
Pole piece, the positive electrode are one of LiFePO4, LiMn2O4, cobalt acid lithium or three metaclass materials, and the binder is fourth
Nitrile rubber NBR, modified polyvinyl chloride TPE, natural rubber NB, Kynoar-hexafluoropropene PVDF-HFP or Kynoar
One of PVDF or a variety of, the conductive agent are one of the black SP of conductive acetylene, carbon pipe or graphene or a variety of, described molten
Agent is NMP.
Compared to conventional liquid lithium ion battery, consolidating based on low temperature flexibility solid polyelectrolyte film prepared by the present invention
State lithium ion battery not only overcomes the drawbacks of battery leakage, but also since the dielectric film has excellent low-temperature flexibility and leads
The advantages that electrical property, is conducive to the popularization and use of solid lithium ion battery at low ambient temperatures.
Polymer solid electrolyte film used in low temperature solid-state lithium ion battery prepared by the present invention has at low temperature
Good conductivity and flexibility, being capable of efficient, stabilization, the solid lithium ion battery recycled safely under low temperature so that preparing
It is possibly realized.
Detailed description of the invention
Fig. 1 is the ionic conductivity figure of the solid electrolyte in embodiment 1 and comparative example；
Fig. 2 is -20 DEG C of low temperature of cycle performance figure of the solid lithium ion battery in embodiment 1 and comparative example.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
The preparation of positive plate:
According to the mass percent of 80:3:7:10, by iron phosphate serving as positive active material, conductive agent acetylene black, lithium salts perchloric acid
Lithium and binder modification polyvinyl chloride TPE are added in appropriate solvent NMP, are tuned into slurry, are coated on aluminium foil after ball milling, so
After be put in baking oven in 80 DEG C of dry 30min, then in vacuum drying oven in 110 DEG C drying obtain positive plate for 24 hours.
The preparation method of low temperature flexibility solid polyelectrolyte film comprises the following steps:
Step S1: modified polyvinyl chloride TPE 2g and lithium salts LiTFSI 1g is taken to be dissolved in appropriate solvents tetrahydrofurane and stirring evenly
Obtain clarification viscous solution；
Step S2: plasticizer phthalic acid diethylester DEP 1g is added in the viscous solution obtained to step S1, is sufficiently stirred
It is uniformly mixed and obtains solution A；
Step S3: by inorganic particle LLZO 1.2g and tetrahydrofuran mixing and ball milling, mixed system B is obtained after fully dispersed；
Step S4: the mixed system B that step S3 is obtained is added in the solution A that step S2 is obtained, is divided after being sufficiently mixed
Granular media system C；
Step S5: the dispersion C that step S4 is obtained is prolonged into stream film forming in silicone oil paper, is put into vacuum drying oven after natural drying
In 60 DEG C of dry 12h, can from silicone oil paper isolated low temperature flexibility solid polyelectrolyte film.
Fig. 1 gives the ionic conductivity figure of low temperature flexibility solid polyelectrolyte film, and test uses occasion China CHI760B
Type electrochemical workstation.
- 20 DEG C of low temperature of the cycle performance figure that Fig. 2 gives solid lithium ion battery passes through the modification system as seen from the figure
Standby solid lithium ion battery shows good low temperature electrochemical performance.
Embodiment 2
The preparation of positive plate:
According to the mass percent of 80:3:7:10, by positive electrode active materials cobalt acid lithium, conductive agent acetylene black, lithium salts lithium perchlorate
It is added in appropriate solvent NMP with binder modification polyvinyl chloride TPE, is tuned into slurry, is coated on aluminium foil after ball milling, so
After be put in baking oven in 80 DEG C of dry 30min, then in vacuum drying oven in 110 DEG C drying obtain positive plate for 24 hours.
The preparation method of low temperature flexibility solid polyelectrolyte film comprises the following steps:
Step S1: modified polyvinyl chloride TPE/ polyvinyl fluoride PVF mixture 2g and lithium salts LiTFSI 0.2g is taken to be dissolved in appropriate solvent
Clarification viscous solution is uniformly mixing to obtain in acetonitrile；
Step S2: being added plasticizer ethylene carbonate EC 0.6g in the viscous solution obtained to step S1, is thoroughly mixed
It is even to obtain solution A；
Step S3: by inorganic particle LLZO 1.2g and tetrahydrofuran mixing and ball milling, mixed system B is obtained after fully dispersed；
Step S4: the mixed system B that step S3 is obtained is added in the solution A that step S2 is obtained, is divided after being sufficiently mixed
Granular media system C；
Step S5: the dispersion C that step S4 is obtained is prolonged into stream film forming in silicone oil paper, is put into vacuum drying oven after natural drying
In 60 DEG C of dry 12h, can from silicone oil paper isolated low temperature flexibility solid polyelectrolyte film.
Comparative example 1
1 difference from Example 1 of comparative example is: without addition modified polyvinyl chloride TPE, the solid-state in solid electrolyte membrane
Dielectric film is unable to normal playback electricity at -20 DEG C.
Fig. 1 gives the ionic conductivity figure of comparative example solid electrolyte film, and test uses occasion China CHI760B type electrochemistry
Work station.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (5)
1. a kind of preparation method of low temperature flexibility solid polyelectrolyte film, it is characterised in that detailed process are as follows: by polymer
It is added in solvent after the plasticizer mixing of the lithium salts and polymer quality 10% ~ 50% of quality 5% ~ 20% and sufficiently dissolves, then will gather
Close amount of substance 10% ~ 90% inorganic particle and solvent mixing and ball milling after be added in above-mentioned solution, acquired solution by blade coating or
Curtain coating is coated on carrier, up to the low temperature flexibility solid polyelectrolyte with a thickness of 20 ~ 100 μm after 60 ~ 120 DEG C of drying
Film；
The polymer is modified polyvinyl chloride TPE or modified polyvinyl chloride TPE and polyvinylchloride, polyvinyl fluoride PVF, gathers
Vinyl chloride PVC, nitrile rubber NBR, modified polyvinyl chloride TPE, natural rubber NB or Kynoar-hexafluoropropene PVDF-HFP
One of or a variety of mixtures；
The lithium salts is LiN (SO2CF3)2(LiTFSI), LiN (SO2F)2(LiFSI), LiB (C2O4)2(LiBOB), LiBC2O4F2
(LiDFOB) or LiClO4One of or it is a variety of；
The plasticizer is succinonitrile (SN), diethyl phthalate (DEP), ethylene carbonate (EC), propene carbonate
(PC), one of polyethylene glycol dimethyl ether (PEGDME) or kaolin or a variety of；
The solvent is N-Methyl pyrrolidone (NMP), acetonitrile, acetone, ethyl acetate, N,N-dimethylformamide (DMF), four
One of hydrogen furans (THF) or dimethyl acetamide (DMAC) are a variety of；
The inorganic particle is LLZO, Al2O3, one of LAGP or LATP or a variety of；
The carrier is one of aluminium foil, copper foil, silicone oil paper or glaxin release paper.
2. the preparation method of low temperature flexibility solid polyelectrolyte film according to claim 1, it is characterised in that: described
Polymer is preferably modified polyvinyl chloride TPE, and the mass ratio of modified polyvinyl chloride TPE and lithium salts is in 10:1 ~ 3, gained low temperature
Flexible polymer solid electrolyte membrane has preferable cryogenic property, and the density of the low temperature flexibility solid polyelectrolyte film is
The half of polychloroethylene film, tensile strength and tearing strength are respectively 20-25MPa and 50-60KN/m, and brittle point is -65 DEG C ~ -75
DEG C, and polychloroethylene film is only the order of magnitude of gained low temperature flexibility solid polyelectrolyte membrane conductivity at -40 DEG C, -15 DEG C
Reach 10-4S/cm。
3. the preparation method of low temperature flexibility solid polyelectrolyte film according to claim 1, it is characterised in that specific
Step are as follows:
Step S1: taking modified polyvinyl chloride TPE 2g and lithium salts LiTFSI 1g to be dissolved in solvents tetrahydrofurane and is stirred
It is even to obtain clarification viscous solution；
Step S2: plasticizer phthalic acid diethylester DEP 1g is added in the viscous solution obtained to step S1, is sufficiently stirred
It is uniformly mixed and obtains solution A；
Step S3: by inorganic particle LLZO 1.2g and tetrahydrofuran mixing and ball milling, mixed system B is obtained after fully dispersed；
Step S4: the mixed system B that step S3 is obtained is added in the solution A that step S2 is obtained, after being sufficiently mixed uniformly
To dispersion C；
Step S5: the dispersion C that step S4 is obtained is prolonged into stream film forming in silicone oil paper, is put into vacuum drying oven after natural drying
In 60 DEG C of dry 12h, then the isolated low temperature flexibility solid polyelectrolyte film from silicone oil paper.
4. low temperature flexibility solid polyelectrolyte film is low made from method described according to claim 1 ~ any one of 3
Application in warm solid Li-ion battery, it is characterised in that detailed process are as follows: by the low temperature flexibility solid polyelectrolyte
The size of film as required is attached on positive plate after cutting, then covers negative electrode tab lithium piece, is then assembled up to low-temperature solid lithium
Ion battery.
5. application according to claim 4, it is characterised in that the specific preparation process of the positive plate are as follows: by positive material
It is added in solvent after material, conductive agent, lithium salts and binder 70 ~ 90:1 in mass ratio ~ 5:4 ~ 10:5 ~ 15 mixing, it is fully dispersed
Anode sizing agent is obtained afterwards, and anode sizing agent is coated on after the aluminium foil with a thickness of 10 ~ 20 μm and is toasted in 100 ~ 120 DEG C up to for assembling
The positive plate of low temperature solid-state lithium ion battery, the positive electrode are in LiFePO4, LiMn2O4, cobalt acid lithium or three metaclass materials
One kind, the binder be nitrile rubber NBR, modified polyvinyl chloride TPE, natural rubber NB, Kynoar-hexafluoropropene
One of PVDF-HFP or Kynoar PVDF or a variety of, the conductive agent are the black SP of conductive acetylene, carbon pipe or graphene
One of or it is a variety of, the solvent be NMP.
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| CN108878798A (en) * | 2017-05-08 | 2018-11-23 | 现代自动车株式会社 | Including the cathode material and preparation method thereof for all-solid-state battery group for preventing the coating layer of diffusion |
| CN110289448A (en) * | 2019-05-22 | 2019-09-27 | 浙江天能能源科技股份有限公司 | A kind of lithium anode and preparation method thereof with artificial constructed SEI film |
| CN110400964A (en) * | 2019-07-31 | 2019-11-01 | 苏州顺创新能源科技有限公司 | A kind of lithium ion battery solid electrolyte membrane |
| CN110504484A (en) * | 2019-08-06 | 2019-11-26 | 河南电池研究院有限公司 | A kind of preparation method and applications of gel state electrolyte film |
| CN111029661A (en) * | 2019-12-26 | 2020-04-17 | 成都新柯力化工科技有限公司 | Ultrathin flexible inorganic solid electrolyte of lithium battery, preparation method and application |
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