CN107394272A - A kind of solid lithium ion battery and preparation method thereof - Google Patents
A kind of solid lithium ion battery and preparation method thereof Download PDFInfo
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- CN107394272A CN107394272A CN201710469989.4A CN201710469989A CN107394272A CN 107394272 A CN107394272 A CN 107394272A CN 201710469989 A CN201710469989 A CN 201710469989A CN 107394272 A CN107394272 A CN 107394272A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—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
- H01M10/0566—Liquid materials
- H01M10/0569—Liquid materials characterised by the solvents
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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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of solid lithium ion battery and preparation method thereof, the solid lithium ion battery, it is characterized in that, it includes the solid electrolyte between positive pole, negative pole, both positive and negative polarity, organic solvent is added dropwise in electrolyte and electrode interface, the contact impedance of electrolyte and electrode interface in solid lithium ion battery is reduced, improves the performance of solid lithium ion battery.Solid lithium ion battery of the present invention and preparation method thereof, it is easy to operate, interface impedance is can obviously reduce, lifts lithium ion solid state battery performance.
Description
Technical field
The present invention relates to field of lithium ion battery, and in particular to a kind of solid lithium ion battery and preparation method thereof.
Background technology
Large-scale energy storage system has become the important component of following intelligent grid, exploitation high-efficiency energy-storage technology for
Utilization ratio, power quality and the promotion regenerative resource extensive use for improving existing electricity generation system have great society and economy
Benefit.Most one of technology of industrialization promotion prospect is electrochemical energy storage technology in energy storage technology, and lithium ion battery is because of it
The features such as in light weight, higher than energy/specific power, long lifespan, is considered as one of electrochemical energy storage technology of most competitiveness, and
Application in each link of energy storage is also more and more extensive.But the lithium rechargeable battery of current large-scale commercial, which generally uses, to be had
The liquid electrolyte of machine carbonates, easy leakage, easy firing, explosive, limits it and further applies.
It is excellent that solid lithium ion battery has that have a safety feature, energy density is high, operating temperature section is wide, has extended cycle life etc.
Put and have been widely recognized, be the study hotspot of field of lithium ion battery.
Up to the present, the conventional electrolyte of solid lithium ion battery mainly includes:Solid polyelectrolyte and inorganic
Solid electrolyte.But because electrolyte is solid-state, no image of Buddha liquid electrolyte equally realizes that electrolyte and the good of electrode connect
Touch, so as to cause the performance of solid lithium ion battery to be significantly worse than the lithium ion battery using liquid electrolyte.
The content of the invention
To solve defect present in above-mentioned prior art, the present invention provides a kind of solid lithium ion battery and its preparation side
Method.
Specifically, the present invention provides a kind of solid lithium ion battery, and it includes the solid-state between positive pole, negative pole, both positive and negative polarity
Electrolyte, organic solvent is added dropwise in electrolyte and electrode interface, reduces electrolyte and electrode interface in solid lithium ion battery
Contact impedance, improve the performance of solid lithium ion battery.
Wherein, the addition of the organic solvent is 10 μ L/cm2-100μL/cm2。
Wherein, described organic solvent be ethylene carbonate, propene carbonate, butylene, vinylene carbonate, 1,
2 ,-dimethyl ethylene carbonate, dimethyl carbonate, diethyl carbonate, dipropyl carbonate, dibutyl carbonate, methyl ethyl carbonate, carbon
Sour first propyl ester, carbonic acid first isopropyl ester, carbonic acid first butyl ester, ethyl propyl carbonic acid ester, ethylene isopropyl ester, ethyl butyl carbonate, in 1,4- fourths
Ester, tetrahydrofuran, dimethyl-tetrahydrofuran, 1,3- dioxolanes, 4- methyl-1,3-dioxies pentamethylene, 1,2- dimethoxys
In ethane, 1,2- diethoxyethane, diglycol ethylene dimethyl ether, contracting TRIGLYME, contracting tetraethyleneglycol dimethyl ether
It is one or more of.
In addition, the active material of the positive pole be cobalt acid lithium, LiFePO4, iron manganese phosphate for lithium, LiMn2O4, nickel ion doped,
One kind in ternary material, ferric sulfate lithium, lithium ion fluorophosphate, lithium vanadium fluorophosphate, lithium iron fluorophosphate, lithium manganese oxide
It is or several;
The active material of described negative pole be lithium metal, lithium metal alloy, graphite, hard carbon, molybdenum disulfide, lithium titanate, graphene,
One or more in antimony oxide, antimony carbon composite, tin antimony composite, Li-Ti oxide;
The electrolyte is solid polyelectrolyte or inorganic solid electrolyte.
In addition, the solid polyelectrolyte is made up of polymer and lithium salts, wherein, lithium salts mass ratio is 10%-60%;
The polymer is polyethylene glycol oxide, polypropylene carbonate, poly- ethylene carbonate, polymerized thylene carbonate vinyl acetate, polymethylacrylic acid
One or more in methyl esters, Kynoar, poly- (biasfluoroethylene-hexafluoropropylene), polyacrylonitrile, polyvinyl alcohol;
The lithium salts is lithium perchlorate, lithium hexafluoro phosphate, dioxalic acid lithium borate, hexafluoroarsenate lithium, LiBF4, trifluoromethyl
At least one of Sulfonic Lithium, bis trifluoromethyl sulfimide lithium and double fluorine sulfimide lithiums.
In addition, the solid polyelectrolyte also inorganic filler containing 1~50wt% and/or fast-ionic conductor.
Wherein, the inorganic filler be silica, titanium dioxide, alundum (Al2O3), zirconium oxide, nickel oxide, silicon nitride,
At least one of magnesium hydroxide, diatomite, montmorillonite and kaolin;The fast-ionic conductor is Li7La3Zr2O12、
Li10GeP2S12、Li3OCl0.5Br0.5、Li3xLa(2/3)-xTiO3、Li5La3Ta2O12、Li5La3Nb2O12、
Li5.5La3Nb1.75In0.25O12、Li3N-LiCl、Li3N-LiBr、Li3N-LiI、Li14Zn(GeO4)4、LiZr2(PO4)3、
Li3OCl, LiPON and Li2S-MaSbAt least one of, wherein, 0 .04<x<0 .14, M=Al, Si or P, a and b value point
Wei 1 ~ 3.
In addition, the inorganic solid electrolyte is Li7La3Zr2O12、Li10GeP2S12、Li3OCl0.5Br0.5、、Li5La3Ta2O12、Li5La3Nb2O12、Li5.5La3Nb1.75In0.25O12、Li3N-LiCl、、Li3N-LiI、Li14Zn(GeO4)4、LiZr2(PO4)3、Li3OCl, LiPON and Li2S-MaSbIn at least one
Kind, wherein, 0 .04<x<0 .14, M=Al, Si or P, a and b value are respectively 1 ~ 3.
The present invention also provides a kind of preparation method of solid lithium ion battery as described above, and it is uniformly applied on electrolyte two sides
Cloth organic solvent, both positive and negative polarity pole piece is separated with the electrolyte, seals to obtain solid lithium ion battery;Described organic solvent is
Ethylene carbonate, propene carbonate, butylene, vinylene carbonate, 1,2 ,-dimethyl ethylene carbonate, carbonic acid diformazan
Ester, diethyl carbonate, dipropyl carbonate, dibutyl carbonate, methyl ethyl carbonate, methyl propyl carbonate, carbonic acid first isopropyl ester, carbonic acid first
Butyl ester, ethyl propyl carbonic acid ester, ethylene isopropyl ester, ethyl butyl carbonate, 1,4- butyrolactone, tetrahydrofuran, dimethyl-tetrahydrofuran, 1,
3- dioxolanes, 4- methyl-1,3-dioxies pentamethylene, 1,2- dimethoxy-ethanes, 1,2- diethoxyethane, contracting diethyl two
One or more in diethylene glycol dimethyl ether, contracting TRIGLYME, contracting tetraethyleneglycol dimethyl ether.
The present invention also provides a kind of method for improving solid lithium ion battery electrolyte/electrode interface, by electrolyte
10 μ L/cm are added dropwise with electrode interface2-100μL/cm2Organic solvent, reduce electrolyte and electrode interface in solid lithium ion battery
Contact impedance, improve the performance of solid lithium ion battery;Described organic solvent is ethylene carbonate, propene carbonate, carbon
Sour butene esters, vinylene carbonate, 1,2 ,-dimethyl ethylene carbonate, dimethyl carbonate, diethyl carbonate, dipropyl carbonate,
Dibutyl carbonate, methyl ethyl carbonate, methyl propyl carbonate, carbonic acid first isopropyl ester, carbonic acid first butyl ester, ethyl propyl carbonic acid ester, ethylene are different
Propyl ester, ethyl butyl carbonate, 1,4- butyrolactone, tetrahydrofuran, dimethyl-tetrahydrofuran, 1,3- dioxolanes, 4- methyl isophthalic acids, 3-
Dioxolanes, 1,2- dimethoxy-ethanes, 1,2- diethoxyethane, diglycol ethylene dimethyl ether, contracting triethylene glycol diformazan
One or more in ether, contracting tetraethyleneglycol dimethyl ether.
Solid lithium ion battery of the present invention and preparation method thereof, it is easy to operate, interface impedance is can obviously reduce, lifts lithium
Ion solid state battery performance.
Brief description of the drawings
Fig. 1 is the impedance contrast figure of embodiment 1 and comparative example 1.
Fig. 2 is 50 DEG C of charging and discharging curves of solid lithium ion battery of embodiment 1.
Embodiment
With reference to being described in detail to the present invention in conjunction with the embodiments, it will be appreciated that preferred embodiment described herein is only
For instruction and explanation of the present invention, it is not intended to limit the present invention.
Battery prepares and performance test:
(1) preparation of positive plate
Kynoar (PVdF) is dissolved in 1-METHYLPYRROLIDONE by A, concentration 5wt.%.
B is by PVdF, conductive charcoal, positive electrode active materials with 10:10:After 80 mass ratio mixing, stir at least 1 hour.
Slurry obtained by upper step is evenly coated on aluminium foil by C, and thickness is 100-120 μm, is first dried at 100 DEG C,
Dried under 120 DEG C of vacuum drying ovens, roll-in, punching, continue to dry in 120 DEG C of vacuum drying ovens after weighing, be put in glove box
In it is standby.
(2) preparation of negative plate
Negative plate is prepared using following steps using metal lithium sheet or negative active core-shell material
PVdF is dissolved in 1-METHYLPYRROLIDONE by A, concentration 5wt.%.
B is by PVdF, conductive charcoal, negative active core-shell material with 10:10:After 80 mass ratio mixing, stir at least 1 hour.
Slurry obtained by upper step is evenly coated on copper foil by C, and thickness is 100-120 μm, is first dried at 100 DEG C,
Dried under 120 DEG C of vacuum drying ovens, roll-in, punching, continue to dry in 120 DEG C of vacuum drying ovens after weighing, be put in glove box
In it is standby.
(3) battery assembles
In electrolyte two sides even spread organic solvent, both positive and negative polarity pole piece is separated with above-mentioned electrolyte, seals all solid state
Lithium ion battery.
(4) battery impedance is tested
Using Autolab electrochemical workstations, in the range of 1MHz-0.1MHz, with 10mV disturbance voltages carry out all solid lithium from
Sub- battery impedance test.
(5) battery charging/discharging performance testing
Charging and discharging curve, multiplying power and the length of all solid state serondary lithium battery at different temperatures are tested with LAND battery charge and discharges instrument to follow
Ring performance.
Embodiment 1
Electrolyte:Poly- ethylene carbonate(Quality:10%)/ poly- (biasfluoroethylene-hexafluoropropylene)(Quality:50%)+ bis trifluoromethyl
Sulfimide lithium(Quality:40%)
Positive electrode active materials:LiFePO4
Negative pole:Lithium metal
Organic solvent:Propene carbonate
Organic solvent coated weight, 10 μ L/cm2
Embodiment 2
Electrolyte:Poly- ethylene carbonate (quality:60%)+lithium perchlorate (quality:40% )
Positive pole:Cobalt acid lithium
Negative pole:Lithium metal
Organic solvent:Ethylene carbonate
Organic solvent coated weight, 100 μ L/cm2
Embodiment 3
Electrolyte:Polyethylene glycol oxide (quality:80%)+lithium perchlorate (quality:20% )
Positive pole:LiMn2O4
Negative pole:Graphite
Organic solvent:Methyl ethyl carbonate
Organic solvent coated weight, 50 μ L/cm2
Comparative example 1
Electrolyte:Poly- ethylene carbonate(Quality:10%)/ poly- (biasfluoroethylene-hexafluoropropylene)(Quality:50%)+ bis trifluoromethyl
Sulfimide lithium(Quality:40%)
Positive pole:LiFePO4
Negative pole:Lithium metal
Organic solvent:Nothing
Comparative example 2
Electrolyte:Poly- ethylene carbonate (quality:60%)+lithium perchlorate (quality:40% )
Positive pole:Cobalt acid lithium
Negative pole:Lithium metal
Organic solvent:Nothing
Comparative example 3
Electrolyte:Polyethylene glycol oxide (quality:80%)+lithium perchlorate (quality:20% )
Positive pole:LiMn2O4
Negative pole:Graphite
Organic solvent:Nothing
Table 1, cell interface impedance test results are as follows:
In addition, Fig. 1 is the impedance contrast figure of embodiment 1 and comparative example 1.Fig. 2 is that 50 DEG C of the solid lithium ion battery of embodiment 1 fills
Discharge curve.From Fig. 1 and Fig. 2, solid lithium ion battery of the invention improves interface impedance, and charge/discharge cycle characteristics
It is good.
Claims (10)
- A kind of 1. solid lithium ion battery, it is characterised in that it includes the solid electrolyte between positive pole, negative pole, both positive and negative polarity, Organic solvent is added dropwise with electrode interface in electrolyte, reduces the contact impedance of electrolyte and electrode interface in solid lithium ion battery, Improve the performance of solid lithium ion battery.
- 2. solid lithium ion battery according to claim 1, it is characterised in that the addition of the organic solvent is。
- 3. solid lithium ion battery according to claim 1 or 2, it is characterised in that described organic solvent is ethylene Alkene ester, propene carbonate, butylene, vinylene carbonate, 1,2 ,-dimethyl ethylene carbonate, dimethyl carbonate, carbonic acid Diethylester, dipropyl carbonate, dibutyl carbonate, methyl ethyl carbonate, methyl propyl carbonate, carbonic acid first isopropyl ester, carbonic acid first butyl ester, carbon Sour second propyl ester, ethylene isopropyl ester, ethyl butyl carbonate, 1,4- butyrolactone, tetrahydrofuran, dimethyl-tetrahydrofuran, 1,3- dioxies Pentamethylene, 4- methyl-1,3-dioxies pentamethylene, 1,2- dimethoxy-ethanes, 1,2- diethoxyethane, diglycol ethylene diformazan One or more in ether, contracting TRIGLYME, contracting tetraethyleneglycol dimethyl ether.
- 4. according to the solid lithium ion battery described in any one in claim 1-3, it is characterised in thatThe active material of the positive pole be cobalt acid lithium, LiFePO4, iron manganese phosphate for lithium, LiMn2O4, nickel ion doped, ternary material, One or more in ferric sulfate lithium, lithium ion fluorophosphate, lithium vanadium fluorophosphate, lithium iron fluorophosphate, lithium manganese oxide;The active material of described negative pole be lithium metal, lithium metal alloy, graphite, hard carbon, molybdenum disulfide, lithium titanate, graphene, One or more in antimony oxide, antimony carbon composite, tin antimony composite, Li-Ti oxide;The electrolyte is solid polyelectrolyte or inorganic solid electrolyte.
- 5. solid lithium ion battery according to claim 4, it is characterised in thatThe solid polyelectrolyte is made up of polymer and lithium salts, wherein, lithium salts mass ratio is 10%-60%;The polymer is polyethylene glycol oxide, polypropylene carbonate, poly- ethylene carbonate, polymerized thylene carbonate vinyl acetate, poly- methyl-prop One or more in e pioic acid methyl ester, Kynoar, poly- (biasfluoroethylene-hexafluoropropylene), polyacrylonitrile, polyvinyl alcohol;The lithium salts is lithium perchlorate, lithium hexafluoro phosphate, dioxalic acid lithium borate, hexafluoroarsenate lithium, LiBF4, trifluoromethyl At least one of Sulfonic Lithium, bis trifluoromethyl sulfimide lithium and double fluorine sulfimide lithiums.
- 6. solid lithium ion battery according to claim 5, it is characterised in that the solid polyelectrolyte also contains 1~50wt% inorganic filler and/or fast-ionic conductor.
- 7. solid lithium ion battery according to claim 6, it is characterised in thatThe inorganic filler be silica, titanium dioxide, alundum (Al2O3), zirconium oxide, nickel oxide, silicon nitride, magnesium hydroxide, At least one of diatomite, montmorillonite and kaolin;The fast-ionic conductor is Li7La3Zr2O12、Li10GeP2S12、Li3OCl0.5Br0.5、Li3xLa(2/3)-xTiO3、 Li5La3Ta2O12、Li5La3Nb2O12、Li5.5La3Nb1.75In0.25O12、Li3N-LiCl、Li3N-LiBr、Li3N-LiI、Li14Zn (GeO4)4、LiZr2( PO4)3、Li3OCl, LiPON and Li2S-MaSbAt least one of, wherein, 0 .04<x<0 .14, M= Al, Si or P, a and b value are respectively 1 ~ 3.
- 8. solid lithium ion battery according to claim 4, it is characterised in that the inorganic solid electrolyte is Li7La3Zr2O12、Li10GeP2S12、Li3OCl0.5Br0.5、Li3xLa(2/3)-xTiO3、Li5La3Ta2O12、Li5La3Nb2O12、 Li5.5La3Nb1.75In0.25O12、Li3N-LiCl、Li3N-LiBr、Li3N-LiI、Li14Zn( GeO4 )4、LiZr2( PO4 )3、 Li3OCl, LiPON and Li2S-MaSbAt least one of, wherein, 0 .04<x<0 .14, M=Al, Si or P, a and b value point Wei 1 ~ 3.
- 9. the preparation method of solid lithium ion battery as described in any one in a kind of 1-8 such as claim, it is characterised in that in electricity Matter two sides even spread organic solvent is solved, both positive and negative polarity pole piece is separated with the electrolyte, seals to obtain solid lithium ion battery;Institute The organic solvent stated be ethylene carbonate, propene carbonate, butylene, vinylene carbonate, 1,2 ,-dimethyl ethylene Alkene ester, dimethyl carbonate, diethyl carbonate, dipropyl carbonate, dibutyl carbonate, methyl ethyl carbonate, methyl propyl carbonate, carbonic acid first Isopropyl ester, carbonic acid first butyl ester, ethyl propyl carbonic acid ester, ethylene isopropyl ester, ethyl butyl carbonate, 1,4- butyrolactone, tetrahydrofuran, diformazan Base tetrahydrofuran, 1,3- dioxolanes, 4- methyl-1,3-dioxies pentamethylene, 1,2- dimethoxy-ethanes, 1,2- diethoxies One or more in ethane, diglycol ethylene dimethyl ether, contracting TRIGLYME, contracting tetraethyleneglycol dimethyl ether.
- A kind of 10. method for improving solid lithium ion battery electrolyte/electrode interface, it is characterised in that:By in electrolyte and 10 μ L/cm are added dropwise in electrode interface2-100μL/cm2Organic solvent, reduce electrolyte and electrode interface in solid lithium ion battery Contact impedance, improve the performance of solid lithium ion battery;Described organic solvent is ethylene carbonate, propene carbonate, carbonic acid Butene esters, vinylene carbonate, 1,2 ,-dimethyl ethylene carbonate, dimethyl carbonate, diethyl carbonate, dipropyl carbonate, carbon Dibutyl phthalate, methyl ethyl carbonate, methyl propyl carbonate, carbonic acid first isopropyl ester, carbonic acid first butyl ester, ethyl propyl carbonic acid ester, ethylene isopropyl Ester, ethyl butyl carbonate, 1,4- butyrolactone, tetrahydrofuran, dimethyl-tetrahydrofuran, 1,3- dioxolanes, 4- methyl isophthalic acids, 3- bis- Oxygen pentamethylene, 1,2- dimethoxy-ethanes, 1,2- diethoxyethane, diglycol ethylene dimethyl ether, contracting TRIGLYME, One or more in contracting tetraethyleneglycol dimethyl ether.
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CN108155412A (en) * | 2017-12-26 | 2018-06-12 | 暨南大学 | A kind of inorganic-inorganic hybrid solid-state electrolyte ceramic membrane and preparation method thereof |
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CN108923060A (en) * | 2018-06-29 | 2018-11-30 | 桑顿新能源科技有限公司 | A kind of solid state lithium battery and preparation method of modifying interface |
CN109473710A (en) * | 2018-12-26 | 2019-03-15 | 清华大学 | A kind of solid state lithium battery with low interfacial resistance |
CN109830643A (en) * | 2019-01-11 | 2019-05-31 | 蜂巢能源科技有限公司 | Reduce the film and its preparation method and application of lithium battery interface impedance |
US20220093967A1 (en) * | 2019-04-17 | 2022-03-24 | University Of Louisville Research Foundation, Inc. | Methods for wet chemical synthesis of lithium argyrodites and enhancing interface stability |
CN110416637A (en) * | 2019-06-28 | 2019-11-05 | 上海空间电源研究所 | A kind of preparation method and applications of solid state battery buffer layer |
CN110416637B (en) * | 2019-06-28 | 2022-08-12 | 上海空间电源研究所 | Preparation method and application of solid-state battery buffer layer |
CN113140788A (en) * | 2021-04-22 | 2021-07-20 | 昆山宝创新能源科技有限公司 | Quasi-solid electrolyte and quasi-solid lithium ion battery |
CN114551998A (en) * | 2022-04-21 | 2022-05-27 | 河南电池研究院有限公司 | Solid-state lithium ion battery and preparation method thereof |
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