CN108288690A - A kind of lithium solid state battery cathode and its preparation method and application - Google Patents
A kind of lithium solid state battery cathode and its preparation method and application Download PDFInfo
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- CN108288690A CN108288690A CN201710012273.1A CN201710012273A CN108288690A CN 108288690 A CN108288690 A CN 108288690A CN 201710012273 A CN201710012273 A CN 201710012273A CN 108288690 A CN108288690 A CN 108288690A
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- cathode
- lithium
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- solid state
- state battery
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
Abstract
The present invention provides a kind of cathode and its preparation method and application of lithium solid state battery, and the cathode includes negative current collector and the negative material that is supported on the negative current collector, wherein the negative material includes：Composite negative electrode active material, conductive additive containing lithium metal and binder.By cathode provided by the invention in lithium solid state battery, the energy density and security performance of lithium ion battery can be improved, and the problems such as material dusting and interfacial contact has been effectively relieved due to the cathode, the lithium solid state battery being prepared into is than using pure metal lithium to have better cycle performance as the lithium solid state battery of cathode.
Description
Technical field
The present invention relates to electrochemistry and novel energy resource material technology field more particularly to a kind of cathode of lithium solid state battery, it is somebody's turn to do
The preparation method of cathode and lithium solid state battery comprising the cathode.
Background technology
Currently, lithium ion battery is the highest battery of energy density in commercial batteries, it is widely used in various small electricals
Sub- product and electric vehicle etc..But in recent years, the energy of fast-developing electric vehicle and energy storage industry to lithium ion battery
More stringent requirements are proposed for metric density and cycle life.In addition, the reason of due to the use of liquid electrolyte, lithium ion battery is being pacified
Full aspect of performance also has much room for improvement always.
In order to solve the problems, such as existing for lithium ion battery currently on the market these, many colleges and universities, scientific research institutions and enterprise are all
Take up the development of propulsion lithium solid state battery.Lithium solid state battery is mainly characterized by, using lithium metal as cathode, greatling improve
The energy density of battery, while solid electrolyte is used, ensure the security performance of battery.But using pure metal lithium as cathode
Lithium solid state battery the problems such as there is also material dusting and interfacial contacts at present, cause the cycle performance of battery poor, it is difficult to practical
Using.
Invention content
The purpose of the present invention is to provide a kind of cathode of novel lithium solid state battery, are substituted pure lithium metal and are used in lithium
In solid state battery, the problems such as material dusting existing for inside battery and interfacial contact is effectively relieved, to improve the cycle of battery
Performance.Meanwhile for lithium ion battery in the market, the lithium solid state battery can improve again battery energy density and
Security performance.
The present invention provides a kind of cathode of lithium solid state battery, the cathode includes negative current collector and is supported on the cathode
Negative material on collector, wherein the negative material includes：Composite negative electrode active material, conductive addition containing lithium metal
Agent and binder.
According to cathode provided by the invention, wherein the composite negative electrode active material containing lithium metal include lithium metal with
The micro- carbon ball of natural graphite, artificial graphite, interphase (MCMB), soft carbon, hard carbon, carbon fiber, porous carbon, carbon black, graphene, carbon are received
Mitron, lithium titanate, nano-silicon, silicon-carbon compound, the sub- silicon of oxidation, the sub- silicon-carbon compound of oxidation, simple substance tin, tin-oxide and tin cobalt
The mixture or compound of one or more compositions in carbon.Wherein, the mixture refer to by physical mechanical mixing will be golden
Category lithium is placed between the particle and particle of other negative electrode active materials or particle surface.The compound refers to by physics or change
Technique is learned to be placed in lithium metal inside the particle of other negative electrode active materials.
According to cathode provided by the invention, wherein the conductive additive includes acetylene black, carbon nanotube, electrically conductive graphite
With it is one or more in carbon fiber.
According to cathode provided by the invention, wherein the binder includes Kynoar, polytetrafluoroethylene (PTFE), acetic acid second
Enester, carboxymethyl cellulose, carboxymethyl cellulose derivative, alginic acid, sodium alginate, polyacrylic acid, Sodium Polyacrylate, polyamides
Amino acid, polyamic acid sodium, polyvinyl alcohol, starch, hydroxypropyl cellulose, hydroxypropyl cellulose sodium, phenolic resin, epoxy resin,
It is one or more in polyimides, polyamidoimide and butadiene-styrene rubber.
According to cathode provided by the invention, wherein the collector can be copper foil, copper mesh, titanium foil, titanium net, stainless steel
Foil, stainless (steel) wire or nickel screen.
According to cathode provided by the invention, wherein described to contain lithium metal relative to the negative material of 100 mass parts
Composite negative electrode active material be 80~99 mass parts, the conductive additive be 0~19 mass parts, the binder be 1~
20 mass parts.Preferably, the negative material relative to 100 mass parts, the composite negative pole active matter containing lithium metal
Matter is 85~95 mass parts, and the conductive additive is 1~5 mass parts, and the binder is 1~10 mass parts.
The present invention also provides the preparation methods of three kinds of cathode.
In the first embodiment, the preparation method includes：Under the protection of inert gas, into oily series solvent according to
Secondary addition binder, conductive additive and the composite negative electrode active material containing lithium metal are coated in afflux body surface after mixing
Face, through drying, roll-in, vacuumize after be prepared into the cathode.
The inert gas includes nitrogen and/or argon gas.
The oil series solvent include one kind in N-Methyl pyrrolidone, toluene, dimethylbenzene, acetone, hexane and heptane or
It is a variety of.
The drying steps refer to drying the pole piece placement for coating slurry in an oven, and temperature is 40~200 DEG C, dry
Time is 20 minutes or more.Preferably, dry temperature is 70~100 DEG C, and drying time is 1~2 hour.
The calandering steps refer to that dried pole piece is carried out roll-in using roll squeezer, and pressure is 1~200000N, excellent
Selection of land, rolling pressure are 100000~150000N.
The vacuum step refers to that the good pole piece of roll-in is placed in vacuum drying oven, in baking oven air pressure be less than or equal to
0.001Mpa, temperature are 100~200 DEG C, and the pumpdown time is 2 hours or more.Preferably, vacuum step air pressure be less than etc.
In 0.00001Mpa, temperature is 100~120 DEG C, and the time is 12~24 hours.
In second of embodiment, the preparation method includes：Binder, conductive additive are added into solvent and removes
Negative electrode active material other than lithium metal is coated in collection liquid surface, again by metal lithium sheet after drying, roll-in after mixing
It is placed in the cathode that the present invention is made in the pole piece.
In the third embodiment, the preparation method includes：Binder, conductive additive are added into solvent and removes
Negative electrode active material other than lithium metal is coated in collection liquid surface, the pole piece is made after drying, roll-in after mixing
Full battery, is used in combination excessive active material containing lithium as the anode of the full battery, and being charged as cathode by battery mends lithium, this is made
The cathode of invention.
The present invention also provides a kind of lithium solid state battery, the lithium solid state battery includes anode, cathode and is located at positive
Electrolyte between cathode, wherein the cathode is cathode provided by the invention or is born according to made from the method for the present invention
Pole.
The anode includes positive active material.The positive active material include LiMn2O4, cobalt acid lithium, LiFePO4,
LiaCobNicMndO2(0.5<a<1.5,0<b<1,0<c<1,0<d<1)、Lia’Nib’Coc’Ald’O2(0.5<a’<1.5,0<b’<1,0
<c’<1,0<d’<1)、Li2MnO3、LiNi0.5Mn1.5O4, sulphur, sulphur carbon complex, lithium sulfide, the oxide of cobalt or sulfide, manganese
Oxide or sulfide, the oxide of nickel or sulfide, the oxide of vanadium or sulfide, molybdenum oxide or sulfide in
The mixture or compound of one or more compositions.
The electrolyte includes polyethylene glycol oxide, polypropylene oxide, poly phosphazene, polysiloxanes, polyacrylonitrile, polyvinylidene fluoride
Alkene, polymethyl methacrylate, Li3xLa2/3-xTiO3(0.04 ＜ X ＜ 0.14), Li3-n(OHn)Cl(0.83≤n≤2)、Li3-n
(OHn)Br(1≤n≤2)、Na1+xZr2P3-xSixO12(0≤X≤3)、Li2+2xZn1-xGeO4(0 ＜ X ＜ 1), Li5La3Ta2O12、
Li5La3Nb2O12、Li3N、Li2S-P2S5And Li2S-SiS2In one or more mixtures or compound.
By cathode provided by the invention in lithium solid state battery, the energy density and safety of lithium ion battery can be improved
Performance, and the problems such as material dusting and interfacial contact has been effectively relieved due to the cathode, the lithium solid state battery ratio being prepared into
Lithium solid state battery using pure metal lithium as cathode has better cycle performance.
Description of the drawings
Hereinafter, carry out the embodiment that the present invention will be described in detail in conjunction with attached drawing, wherein：
Fig. 1 is that lithium solid state battery capacity retention ratio made from the embodiment of the present invention 1 and comparative example 1 is bent with cycle cycle variation
Line chart.
Specific implementation mode
The present invention is further described in detail With reference to embodiment, the embodiment provided is only for explaining
The bright present invention, the range being not intended to be limiting of the invention.
Embodiment 1
It is mixed by physical mechanical, by metallic lithium powder and silicon-carbon cathode material in mass ratio 1:1 is prepared into after mixing
Composite negative pole material containing lithium metal.Then, in argon gas atmosphere, 0.5g Kynoar is taken to be placed in 10gN- crassitudes
It in ketone, using magnetic stirrer 1h or so, waits being completely dissolved, 0.2g conductive additive acetylene blacks is added, continue to stir 1h,
Then composite negative pole materials of the 9.3g containing lithium metal is added, after being stirred for 4h, obtained slurry is coated on copper foil, thickness
It is 200 μm.It is subsequently placed in 80 DEG C of convection ovens and dries, carry out roll-in with the pressure of 100000N, then punching claims piece, finally exists
Vacuum preserves for 24 hours in 120 DEG C of vacuum drying ovens, is then transferred in glove box, is anode with cobalt acid lithium, polyethylene glycol oxide is electrolyte
It is assembled into lithium solid state battery, stands 12h.
The mass energy density that the lithium solid state battery can be obtained after testing is 320Wh/kg, and 100 weeks capacity retention ratios of cycle are
81%.Its capacity retention ratio is shown in attached drawing 1 with cycle cycle change curve.
Embodiment 2
First, 0.5g Kynoar is taken to be placed in 10gN- methyl pyrrolidones, it is left using magnetic stirrer 1h
The right side waits being completely dissolved, and 0.2g conductive additive acetylene blacks are added, and continues to stir 1h, and 9.3g silicon-carbon cathode materials are then added, then
After stirring 4h, obtained slurry is coated on copper foil, thickness is 200 μm.It is subsequently placed in 80 DEG C of convection ovens and dries, use
The pressure of 100000N carries out roll-in, then punching claims piece, and finally vacuum preserves for 24 hours in 120 DEG C of vacuum drying ovens, retransfers in one's hands
It is assembled in casing.In an assembling process, a piece of thin lithium piece is placed again in the silicon-carbon cathode pole piece prepared, it is whole to make
For cathode, and it is anode with cobalt acid lithium, polyethylene glycol oxide is electrolyte, is assembled into lithium solid state battery, stands 12h.
The mass energy density that the lithium solid state battery can be obtained after testing is 315Wh/kg, and 100 weeks capacity retention ratios of cycle are
80%.
Embodiment 3
First, 0.5g Kynoar is taken to be placed in 10gN- methyl pyrrolidones, it is left using magnetic stirrer 1h
The right side waits being completely dissolved, and 0.2g conductive additive acetylene blacks are added, and continues to stir 1h, and 9.3g silicon-carbon cathode materials are then added, then
After stirring 4h, obtained slurry is coated on copper foil, thickness is 200 μm.It is subsequently placed in 80 DEG C of convection ovens and dries, use
The pressure of 100000N carries out roll-in, then punching claims piece, and finally vacuum preserves for 24 hours in 120 DEG C of vacuum drying ovens, retransfers in one's hands
It is anode with excessive cobalt acid lithium in casing, polyethylene glycol oxide is electrolyte, is assembled into lithium solid state battery, stands 12h.
The mass energy density that the lithium solid state battery can be obtained after testing is 308Wh/kg, and 100 weeks capacity retention ratios of cycle are
78%.
Embodiment 4
First, 0.5g Kynoar is taken to be placed in 10gN- methyl pyrrolidones, it is left using magnetic stirrer 1h
The right side waits being completely dissolved, and 0.2g conductive additive acetylene blacks are added, and continues to stir 1h, and 9.3g silicon-carbon cathode materials are then added, then
After stirring 4h, obtained slurry is coated on copper foil, thickness is 200 μm.It is subsequently placed in 80 DEG C of convection ovens and dries, use
The pressure of 100000N carries out roll-in, then punching claims piece, and finally vacuum preserves for 24 hours in 120 DEG C of vacuum drying ovens, retransfers in one's hands
In casing, Li is first then added in cobalt acid lithium2MnO3Or Li2FeO2As anode additive, keep the amount containing lithium of anode excessive,
Generally positive with this again, polyethylene glycol oxide is electrolyte, is assembled into lithium solid state battery, stands 12h.
The mass energy density that the lithium solid state battery can be obtained after testing is 310Wh/kg, and 100 weeks capacity retention ratios of cycle are
79%.
Comparative example 1
In glove box, using metal lithium sheet as cathode, cobalt acid lithium is anode, and polyethylene glycol oxide is assembled into lithium for electrolyte and consolidates
State battery stands 12h.The mass energy density that the lithium solid state battery can be obtained after testing is 350Wh/kg, recycles 100 weeks capacity and protects
Holdup is 21%.
Its capacity retention ratio is shown in attached drawing 1 with cycle cycle change curve.
This lithium solid-state electricity provided by the invention is can be seen that by the curve comparison of embodiment in Fig. 11 and comparative example 1
The cathode in pond can significantly improve the cycle performance of lithium solid state battery.
Claims (11)
1. a kind of cathode of lithium solid state battery, the cathode includes negative current collector and the cathode that is supported on the negative current collector
Material, wherein the negative material includes：Composite negative electrode active material, conductive additive containing lithium metal and binder.
2. cathode according to claim 1, wherein the composite negative electrode active material containing lithium metal include lithium metal with
The micro- carbon ball of natural graphite, artificial graphite, interphase, soft carbon, hard carbon, carbon fiber, porous carbon, carbon black, graphene, carbon nanotube,
In lithium titanate, nano-silicon, silicon-carbon compound, the sub- silicon of oxidation, the sub- silicon-carbon compound of oxidation, simple substance tin, tin-oxide and tin cobalt carbon
One or more compositions mixture or compound.
3. cathode according to claim 1 or 2, wherein the conductive additive includes acetylene black, carbon nanotube, conduction
It is one or more in graphite and carbon fiber.
4. cathode according to any one of claim 1 to 3, wherein the binder includes Kynoar, polytetrafluoro
Ethylene, vinylacetate, carboxymethyl cellulose, carboxymethyl cellulose derivative, alginic acid, sodium alginate, polyacrylic acid, poly- third
Olefin(e) acid sodium, polyamic acid, polyamic acid sodium, polyvinyl alcohol, starch, hydroxypropyl cellulose, hydroxypropyl cellulose sodium, phenol tree
It is one or more in fat, epoxy resin, polyimides, polyamidoimide and butadiene-styrene rubber.
5. cathode according to any one of claim 1 to 4, wherein the collector is copper foil, copper mesh, titanium foil, titanium
Net, stainless steel foil, stainless (steel) wire or nickel screen.
6. cathode according to any one of claim 1 to 5, wherein relative to the negative material of 100 mass parts,
The composite negative electrode active material containing lithium metal is 80~99 mass parts, and the conductive additive is 0~19 mass parts, described
Binder is 1~20 mass parts；Preferably, relative to the negative material of 100 mass parts, the Compound Negative containing lithium metal
Pole active material is 85~95 mass parts, and the conductive additive is 1~5 mass parts, and the binder is 1~10 mass parts.
7. the preparation method of any one of claim 1 to 6 cathode, this method include：Under the protection of inert gas, to
Binder, conductive additive and the composite negative electrode active material containing lithium metal are sequentially added in oily series solvent, are applied after mixing
Overlay on collection liquid surface, through drying, roll-in, vacuumize after be prepared into the cathode.
8. preparation method according to claim 7, wherein the inert gas includes nitrogen and/or argon gas, it is preferable that
The oil series solvent includes one or more in N-Methyl pyrrolidone, toluene, dimethylbenzene, acetone, hexane and heptane.
9. the preparation method of any one of claim 1 to 6 cathode, this method include：Binder is added into solvent, leads
Electric additive and the negative electrode active material in addition to lithium metal are coated in collection liquid surface, after drying, roll-in after mixing
Metal lithium sheet is placed in the cathode that the present invention is made in the pole piece again.
10. the preparation method of any one of claim 1 to 6 cathode, this method include：Into solvent be added binder,
Conductive additive and the negative electrode active material in addition to lithium metal are coated in collection liquid surface, through drying, roll-in after mixing
Full battery is made in the pole piece afterwards, excessive active material containing lithium is used in combination to be charged as by battery as the anode of the full battery
Cathode mends lithium, and the cathode of the present invention is made.
11. a kind of lithium solid state battery, the lithium solid state battery includes anode, cathode and the electrolysis between anode and cathode
Matter, wherein the cathode is for cathode according to any one of claims 1 to 6 or according to any one of claim 7 to 10
Cathode made from the method.
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| CN201710012273.1A CN108288690B (en) | 2017-01-09 | 2017-01-09 | Lithium solid-state battery cathode and preparation method and application thereof |
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| CN201710012273.1A CN108288690B (en) | 2017-01-09 | 2017-01-09 | Lithium solid-state battery cathode and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109037679A (en) * | 2018-08-01 | 2018-12-18 | 桑德集团有限公司 | Petroleum coke base porous carbon materials and preparation method thereof and silicon-carbon cathode material |
| CN109738823A (en) * | 2018-12-29 | 2019-05-10 | 中国科学院物理研究所 | Method for testing and evaluating the electrolyte system performance of silicon-based anode half-cell |
| CN111509204A (en) * | 2020-04-20 | 2020-08-07 | 中国科学院宁波材料技术与工程研究所 | Preparation method of metal lithium composite negative electrode |
| CN112038579A (en) * | 2020-09-28 | 2020-12-04 | 合肥国轩高科动力能源有限公司 | Metal lithium composite electrode, preparation method thereof and electrochemical energy storage device |
| CN113948674A (en) * | 2021-10-28 | 2022-01-18 | 郑州中科新兴产业技术研究院 | Safe lithium supplement negative plate, preparation method and lithium battery |
| WO2023046089A1 (en) * | 2021-09-26 | 2023-03-30 | 珠海冠宇电池股份有限公司 | Negative electrode plate and lithium-ion battery comprising negative electrode plate |
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