CN108923060A - A kind of solid state lithium battery and preparation method of modifying interface - Google Patents
A kind of solid state lithium battery and preparation method of modifying interface Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H01M10/00—Secondary cells; Manufacture thereof
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- H—ELECTRICITY
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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Abstract
The present invention discloses a kind of solid state lithium battery of modifying interface, including anode composite, lithium anode and solid electrolyte, and the side of solid electrolyte and anode composite are combined closely, and the other side and lithium anode are combined closely by high concentration lithium salts-acetonitrile solution;Anode composite is provided with plus plate current-collecting body, and lithium anode is provided with negative current collector;A kind of preparation method of the solid state lithium battery of modifying interface is also disclosed, including prepares anode composite, prepares solid electrolyte, assembles lithium anode, wherein lithium anode is soaked with high concentration lithium salts-acetonitrile solution, is finally prepared into solid state lithium battery.The present invention can improve the ionic conductivity in anode, be conducive to the interface impedance for reducing anode, cathode and solid electrolyte, and solid state lithium battery multiplying power at room temperature and cycle performance are all improved.
Description
Technical field
The invention belongs to battery technology fields, are related to the solid state lithium battery and preparation method of a kind of modifying interface.
Background technique
Under the background of energy crisis and environmental problem, countries in the world, which all propose fuel-engined vehicle, to be started to be forbidden to use
Time develops new-energy automobile, if electric car (EV) or hybrid vehicle (HEV) have been the task of top priority.Existing lithium
Ion battery uses organic liquid electrolytes, with the problem inflammable, electrochemical window is lower, causes people to electric car
The anxiety of mileage and security performance.Solid electrolyte is due to non-combustible, high electrochemical window, potential substitution liquid electrolyte
Develop solid state lithium battery, while improving the energy density and safety of battery, is to realize that lithium battery energy density is greater than 300Wh/
One of preferred option of kg.
But be solid-solid point contact entirely between solid electrolyte and electrode at present, it is bad that there are interfacial contacts, interface resistance
Resist big problem.Meanwhile the internal infiltration due to lacking electrolyte of anode, ion transmission performance is also poor, therefore solid state battery
Can only again (60 DEG C or more) of high temperature work, can not be in working and room temperature.In addition, solid electrolyte usually with metal lithium electrode wellability
It is poor, need complicated interface-modifying layer.
Patent CN107248591A uses thin-film technique such as electron beam evaporation, magnetron sputtering, arteries and veins in solid electrolyte two sides
The methods of impulse light deposition (PLD) grow nano thickness anode, thin-film technique interfacial contact is preferable, at the same thickness of electrode compared with
It is thin, the solid state lithium battery that cycle performance is excellent at room temperature can be obtained.But this method can not obtain large capacity solid state lithium battery,
Simultaneously using thin-film technique is very time-consuming, is difficult to large-scale production.
Patent CN103904360A grows non-crystal silicic acid on garnet-type solid electrolyte surface using PLD technique
The decorative layer as anode and solid electrolyte such as lithium, lithium sulfate can improve anode and solid electrolytic since amorphous layer is softer
Interfacial contact between matter, but it is unable to improve lithium ion transport performance inside anode, therefore high rate performance nevertheless suffers from limitation.
Active pole piece and sulfide solid electrolyte are heat-treated 1 at 200 DEG C~1000 DEG C by patent CN103972464A
~20h obtains anode composite, is then cold-pressed and pole piece is made on a current collector.Although this method can improve the ion of anode
Conductivity, but it is unable to improve the interface impedance of anode composite/between cathode and solid electrolyte.
Summary of the invention
The present invention is standby using solid anode composite and electrolyte integration system, is made using lithium salts-acetonitrile solution of high concentration
For the interface-modifying layer of lithium anode and electrolyte, ionic resistance inside anode and electrode/electrolyte interface are reduced
Ionic resistance.
A kind of solid state lithium battery of modifying interface, including anode composite, lithium anode and solid electrolyte, the solid
The side of electrolyte and anode composite are combined closely, and the other side and lithium anode pass through the high concentration lithium salts-of 5mol/L or more
Acetonitrile solution is combined closely;The anode composite is provided with plus plate current-collecting body, and the lithium anode is provided with negative current collector.
Further, the anode composite with a thickness of 10~100 μm, the solid electrolyte with a thickness of 20~40 μ
m。
A kind of preparation method of the solid state lithium battery of modifying interface, includes the following steps:
(1) anode composite is prepared:Active material, conductive agent, polymer and lithium salts are uniformly mixed in organic solvent, so
After be uniformly coated on plus plate current-collecting body, dry and be compacted;
(2) solid electrolyte is prepared:Will be evenly dispersed in polymer and lithium ion conductor addition organic solvent, then spread out
On the anode composite of step (1) preparation, drying obtains solid electrolyte;
(3) lithium anode is assembled:Lithium anode one is soaked with high concentration lithium salts-acetonitrile solution of 5mol/L or more
Lithium anode after wetting is put on the solid electrolyte of step (2) preparation, is prepared into solid state lithium battery by side.
Further, the active material is LiFePO4, iron manganese phosphate for lithium, cobalt acid lithium, nickle cobalt lithium manganate, nickel cobalt aluminic acid
Lithium, LiMn2O4, nickel ion doped and lithium-rich manganese base material more than one.
Further, the conductive agent is conductive black, electrically conductive graphite, carbon nanotube, carbon nano-fiber and graphene
More than one.
Further, the polymer be polyethylene glycol oxide, polyacrylonitrile, polymethyl methacrylate, Kynoar,
Polycarbonate-based and polysiloxane-based more than one.
Further, the lithium salts is LiPF6、LiClO4、LiAsF6、LiBF4、LiCF3SO3、LiN(CF3SO2)2、LiB
(C2O4)2And LiBF2(CO2)2More than one, the lithium ion conductor is Li-La-Ti oxygen, Li1+xAlxTi2-x(PO4)3、Li1+ xAlxGe2-x(PO4)3And Li7-xLa3Zr2-xTaxO12More than one, and 0 x≤1 <.
Further, the organic solvent is acetonitrile or N- methyl-pyrrolidon.
Further, the mass ratio of polymer described in step (1) and lithium salts is 1:1~1:3;The active material is led
Electric agent, polymer+lithium salts three mass ratio are x:y:(100-x-y), and 30≤x≤70,5≤y≤15.
Further, the mass ratio of polymer described in step (2) and lithium ion conductor is 1:1~1:3.
Beneficial effects of the present invention:
The solid state lithium battery of modifying interface of the present invention can improve the ionic conductance in anode using anode composite
Rate.Solid electrolyte solution is spread out on anode composite and dried, it is standby using integration system, be conducive to reduce anode/solid
Electrolyte interface impedance.
Lithium anode side is soaked using lithium salts-acetonitrile solution liquid of high concentration, as lithium anode and electrolyte
Interface-modifying layer, be conducive to reduce lithium anode/solid electrolyte interface impedance.
The lithium ion conductor that solid electrolyte uses is by the Li of aluminium, tantalum doping1+xAlxTi2-x(PO4)3、Li1+ xAlxGe2-x(PO4)3And Li7-xLa3Zr2-xTaxO12, be conducive to the conductivity for improving solid electrolyte.
The solid state lithium battery of modifying interface of the present invention multiplying power at room temperature and cycle performance are all improved.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 is the solid state lithium battery structural schematic diagram of modifying interface of the invention;
The nyquist diagram of impedance at Fig. 2 is 30 DEG C of solid state lithium battery of comparative example of the present invention and embodiment 1;
Fig. 3 is the charging and discharging curve of solid state lithium battery different multiplying at 30 DEG C of the modifying interface of the embodiment of the present invention 1
Figure;
Fig. 4 is the solid state lithium battery of comparative example of the present invention in 30 DEG C and the first charge-discharge curve graph of 0.1C;
Fig. 5 is the solid state lithium battery of the modifying interface of the embodiment of the present invention 1 in 30 DEG C and the cycle performance figure of 0.1C;
Fig. 6 is the nyquist diagram of solid state lithium battery impedance at 30 DEG C of the modifying interface of the embodiment of the present invention 2;
Fig. 7 be the embodiment of the present invention 2 modifying interface solid state lithium battery at 30 DEG C electrochemistry high rate performance figure;
Fig. 8 is the solid state lithium battery of the modifying interface of the embodiment of the present invention 2 in 30 DEG C and the cycle performance figure of 0.1C;
Appended drawing reference in above-mentioned figure:
1, negative current collector, 2, lithium anode, 3, lithium salts-acetonitrile solution, 4, solid electrolyte, 5, anode composite, 6,
Plus plate current-collecting body.
Specific embodiment
The following further describes the present invention with reference to the drawings, but is not intended to limit the scope of the invention.
Such as Fig. 1, the present invention provides a kind of solid state lithium battery of modifying interface, including anode composite 5,2 and of lithium anode
Solid electrolyte 4, the side of the solid electrolyte 4 and anode composite 5 are combined closely, and the other side and lithium anode 2 pass through
High concentration lithium salts-acetonitrile solution 3 of 5mol/L or more is combined closely;The anode composite 5 is provided with plus plate current-collecting body 6, described
Lithium anode 2 is provided with negative current collector 1.
As a preferred embodiment, the anode composite 5 with a thickness of 10~100 μm, the solid electrolyte 4 with a thickness of
20~40 μm.
Using anode composite 5, be conducive to improve the ionic conductivity in anode;Solid electrolyte 4 is spread out in anode composite 5
On combine closely, be conducive to reduce anode/solid electrolyte interface impedance;Lithium salts-acetonitrile solution 3 as lithium anode 2 with
The interface-modifying layer of solid electrolyte 4 is conducive to reduce lithium metal/solid electrolyte interface impedance.
The present invention also provides a kind of preparation method of the solid state lithium battery of modifying interface, by following specific embodiments and right
Ratio and attached drawing illustrate.
Comparative example
The preparation method of the solid state lithium battery of comparative example carries out according to the following steps:
(1) Kynoar is dissolved in N- methyl-pyrrolidon in glove box and is stirred for 24 hours, then by itself and phosphorus
Sour iron lithium, LiN (CF3SO2)2, carbon nano-fiber be added in mortar, wherein LiFePO4:Carbon nano-fiber:Kynoar:
LiN(CF3SO2)2Mass ratio be 50:10:10:30, it is fully ground 1h, is uniformly mixed it, slurry is uniformly coated on positive collection
On fluid, drying compacting.
(2) by Li in glove box6.4La3Zr1.4Ta0.6O12With polyethylene glycol oxide (molecular weight:106G/mol) in mass ratio
3:1(Li6.4La3Zr1.4Ta0.6O12Volume fraction be about 12.7vol%) be dissolved in acetonitrile, ultrasonic disperse, and stir for 24 hours
Obtain Li6.4La3Zr1.4Ta0.6O12The evenly dispersed viscous paste of powder.The slurry is uniformly applied on anode composite, to solvent
Acetonitrile volatilization completely, obtains solid electrolyte, anode composite/solid electrolyte interface cohesion is close.
(3) lithium anode side is pressed on solid electrolyte layer, is assembled into solid state lithium battery.
Embodiment 1
The preparation method of the solid state lithium battery of 1 modifying interface of the present embodiment carries out according to the following steps:
(1) Kynoar is dissolved in N- methyl-pyrrolidon in glove box and is stirred for 24 hours, then by itself and phosphorus
Sour iron lithium, LiN (CF3SO2)2, carbon nano-fiber be added in mortar, LiFePO4:Carbon nano-fiber:Kynoar:LiN
(CF3SO2)2Mass ratio be 50:10:10:30, it is fully ground 1h, is uniformly mixed it, slurry is uniformly coated on anode collection
On body, drying compacting.
(2) by Li in glove box6.4La3Zr1.4Ta0.6O12With polyethylene glycol oxide (molecular weight:106G/mol) in mass ratio
3:1(Li6.4La3Zr1.4Ta0.6O12Volume fraction be about 12.7vol%) be dissolved in acetonitrile, ultrasonic disperse, and stir for 24 hours
Obtain Li6.4La3Zr1.4Ta0.6O12The evenly dispersed viscous paste of powder.The slurry is applied on anode composite, to solvent acetonitrile
Volatilization completely, obtains solid electrolyte, anode composite/solid electrolyte interface cohesion is close.
(3) LiN (CF for being 10mol/L with the micro concentration of 5 μ L3SO2)2Acetonitrile solution soak lithium anode side,
Guarantee lithium anode boundary moisture, the side of wetting is pressed on solid electrolyte layer, solid state lithium battery is assembled into.
Solid state lithium battery prepared by comparative example and embodiment 1 carries out the measurement of battery impedance, nyquist diagram such as Fig. 2 institute
Show, passes through the LiN (CF of 10mol/L3SO2)2Acetonitrile solution modification after, solid state lithium battery is in 30 DEG C of impedance by 7000 ohm
It is reduced to less than 1000 ohm, lithium anode and solid electrolyte interface impedance reduce, so that total impedance is obviously reduced.
The charging and discharging curve of solid state lithium battery different multiplying at 30 DEG C prepared by embodiment 1 is as shown in figure 3, comparative example system
The charging and discharging curve of standby solid state lithium battery 0.1C multiplying power at 30 DEG C is as shown in figure 4, the solid state lithium battery through modifying interface exists
Capacity under 0.1C multiplying power reaches 130mAh/g, and capacity reaches 100mAh/g under the multiplying power of 1C, and inornate solid-state lithium is electric
Pond capacity only about 50mAh/g under 0.1C multiplying power, solid state lithium battery can not almost work at 30 DEG C when interface is without polishing.
Solid state lithium battery prepared by embodiment 1 is in 30 DEG C and the cycle performance of 0.1C as shown in figure 5, consolidating through modifying interface
State lithium battery recycles 50 circles under 0.1C multiplying power, and capacity retention ratio 81% has good cycle performance.
Embodiment 2
The preparation method of the solid state lithium battery of 2 modifying interface of the present embodiment carries out according to the following steps:
(1) polycarbonate is dissolved in N- methyl-pyrrolidon in glove box and is stirred for 24 hours, then by itself and nickel cobalt
LiMn2O4 (NCM622), LiN (CF3SO2)2, carbon nanotube be added in mortar, nickle cobalt lithium manganate:Carbon nanotube:Polycarbonate:
LiN(CF3SO2)2Mass ratio be 50:10:15:15, it is fully ground 1h, is uniformly mixed it, slurry is uniformly coated on positive collection
On fluid, drying compacting.
(2) by Li in glove box6.4La3Zr1.4Ta0.6O12With polyethylene glycol oxide (molecular weight:106G/mol) in mass ratio
3:1(Li6.4La3Zr1.4Ta0.6O12Volume fraction be about 12.7vol%) be dissolved in acetonitrile, ultrasonic disperse, and stir for 24 hours
Obtain Li6.4La3Zr1.4Ta0.6O12The evenly dispersed viscous paste of powder.The slurry is applied on anode composite, to solvent acetonitrile
Volatilization completely, obtains solid electrolyte, anode composite/solid electrolyte interface cohesion is close.
(3) LiCF for being 10mol/L with the micro concentration of 5 μ L3SO3Acetonitrile solution soak lithium anode side, guarantee
The side of wetting is pressed on solid electrolyte layer, is assembled into solid state lithium battery by lithium anode boundary moisture.
Solid state lithium battery prepared by embodiment 2 carries out the measurement of battery impedance, nyquist diagram as shown in fig. 6, through
The LiCF of 10mol/L3SO3Acetonitrile solution modification after solid state lithium battery in 30 DEG C of impedance be only 700 ohm, lithium metal is negative
Pole and solid electrolyte interface impedance reduce, so that total impedance is obviously reduced.
Embodiment 2 prepare solid state lithium battery at 30 DEG C electrochemistry high rate performance as shown in fig. 7, consolidating through modifying interface
Capacity of the state lithium battery under 0.1C multiplying power reaches 150mAh/g, and capacity reaches 100mAh/g under the multiplying power of 1C.
Solid state lithium battery prepared by embodiment 2 is in 30 DEG C and the cycle performance of 0.1C as shown in figure 8, consolidating through modifying interface
State lithium battery recycles 50 circles under 0.1C multiplying power, and capacity retention ratio 72% has good cycle performance.
The foregoing describe basic principles and main features of the invention and advantages of the present invention.The technical staff of the industry answers
The understanding, the present invention is not limited to the above embodiments, and the above embodiments and description only describe of the invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these change and change
Into all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent
It defines.
Claims (10)
1. a kind of solid state lithium battery of modifying interface, which is characterized in that including anode composite, lithium anode and solid electrolytic
Matter, the side of the solid electrolyte and anode composite are combined closely, and the other side and lithium anode pass through 5mol/L's or more
High concentration lithium salts-acetonitrile solution is combined closely;The anode composite is provided with plus plate current-collecting body, and the lithium anode is provided with
Negative current collector.
2. the solid state lithium battery of modifying interface according to claim 1, which is characterized in that the anode composite with a thickness of 10
~100 μm, the solid electrolyte with a thickness of 20~40 μm.
3. a kind of preparation method of the solid state lithium battery of modifying interface as described in claim 1, which is characterized in that including walking as follows
Suddenly:
(1) anode composite is prepared:Active material, conductive agent, polymer and lithium salts are uniformly mixed in organic solvent, then
It is even to be coated on plus plate current-collecting body, it dries and is compacted;
(2) solid electrolyte is prepared:Will be evenly dispersed in polymer and lithium ion conductor addition organic solvent, it then spreads out in step
Suddenly on the anode composite of (1) preparation, drying obtains solid electrolyte;
(3) lithium anode is assembled:Lithium anode side is soaked with high concentration lithium salts-acetonitrile solution of 5mol/L or more, it will
Lithium anode after wetting is put on the solid electrolyte of step (2) preparation, is prepared into solid state lithium battery.
4. the preparation method of solid state lithium battery according to claim 3, which is characterized in that the active material is ferric phosphate
Lithium, iron manganese phosphate for lithium, cobalt acid lithium, nickle cobalt lithium manganate, nickel cobalt lithium aluminate, LiMn2O4, nickel ion doped and lithium-rich manganese base material one
Kind or more.
5. the preparation method of solid state lithium battery according to claim 3, which is characterized in that the conductive agent be conductive black,
Electrically conductive graphite, carbon nanotube, carbon nano-fiber and graphene more than one.
6. the preparation method of solid state lithium battery according to claim 3, which is characterized in that the polymer is polyoxyethylene
Alkene, polyacrylonitrile, polymethyl methacrylate, Kynoar, polycarbonate-based and polysiloxane-based more than one.
7. the preparation method of solid state lithium battery according to claim 3, which is characterized in that the lithium salts is LiPF6、LiClO4、
LiAsF6、LiBF4、LiCF3SO3、LiN(CF3SO2)2、LiB(C2O4)2And LiBF2(CO2)2More than one, the lithium ion is led
Body is Li-La-Ti oxygen, Li1+xAlxTi2-x(PO4)3、Li1+xAlxGe2-x(PO4)3And Li7-xLa3Zr2-xTaxO12More than one, and
0 x≤1 <.
8. the preparation method of solid state lithium battery according to claim 3, which is characterized in that the organic solvent be acetonitrile or
N- methyl-pyrrolidon.
9. the preparation method of solid state lithium battery according to claim 3, which is characterized in that polymer described in step (1) and
The mass ratio of lithium salts is 1:1~1:3;The active material, conductive agent, polymer+lithium salts three mass ratio are x:y:(100-
X-y), and 30≤x≤70,5≤y≤15.
10. the preparation method of solid state lithium battery according to claim 9, which is characterized in that polymer described in step (2) and
The mass ratio of lithium ion conductor is 1:1~1:3.
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Cited By (5)
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CN109786842A (en) * | 2018-12-26 | 2019-05-21 | 中国电子科技集团公司第十八研究所 | A kind of high safety high-energy-density lithium/fluorocarbons battery preparation method |
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 |
CN112670543A (en) * | 2020-09-08 | 2021-04-16 | 华中科技大学 | Composite solid electrolyte membrane based on hollow MOF (metal organic framework) and preparation method and application thereof |
CN113410437A (en) * | 2021-06-04 | 2021-09-17 | 天津中电新能源研究院有限公司 | Negative electrode surface protection method suitable for solid lithium battery and secondary lithium battery |
CN113823768A (en) * | 2021-08-27 | 2021-12-21 | 天津空间电源科技有限公司 | Preparation method of positive electrode suitable for solid-state battery |
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