CN106450488B - A kind of in-situ preparation method of the lithium-sulfur cell based on silicium cathode - Google Patents
A kind of in-situ preparation method of the lithium-sulfur cell based on silicium cathode Download PDFInfo
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Abstract
The present invention discloses a kind of in-situ preparation method of lithium-sulfur cell based on silicium cathode.After the present invention is by preparing three electrode lithium sulphur laminated batteries according to positive pole plate of lithium-sulfur cell, lithium/copper metal compound electric pole piece, silicon electrode piece and lithium/copper metal compound electric pole piece lamination sequence, pre- storage lithium is carried out to silicon electrode piece using the method for pre- storage lithium in situ, after pre- storage lithium, lithium/copper metal compound electric pole piece is taken out and is encapsulated in situ, is obtained using silicon electrode piece as the lithium-sulfur cell of cathode.This process simplify the preparation process flow of silicon substrate lithium-sulfur cell, saves and tear battery open, takes pole piece and repeat the process of film-making, evaded the failure risk of prior art, be easily converted into industrial production technology.
Description
Technical field
The invention belongs to lithium-sulfur cell technical fields, are related to a kind of side of being prepared in situ of lithium-sulfur cell based on silicium cathode
Method.
Background technique
Lithium-sulfur cell is a kind of secondary chemical sources of electric energy of high-energy density, with consumer electronics product, new-energy automobile
And the fast development in the fields such as energy-storage system, lithium-sulfur cell are concerned.The specific capacity of sulphur anode is up to 1675mAh/g, much
Higher than the material of commercial widely applied cobalt acid lithium battery.The theoretical specific capacity of lithium metal is 3860mAh/g, lithium-sulfur cell reason
It is up to 2600Wh/kg by energy density, and sulphur is a kind of environment amenable element, is not polluted substantially to environment, considered
To sulphur, cost is relatively low, so, lithium-sulfur cell has extraordinary application prospect in next-generation power battery.
Lithium-sulfur cell, which uses, has sulphur-sulfide linkage sulfur-based compound as a positive electrode active material, and the polysulfide of lithium is molten
It in electrolyte, reacts with the lithium an- ode of high activity, easily causes shuttle effect, active material is caused to lose, cause certainly
Electric discharge, influences cycle performance.
Lithium-sulfur cell generally uses metallic lithium foil to do cathode, lithium metal chemical reactivity with higher, chemistry shakiness
It is fixed, it is more with sulfur-based compound side reaction, generate self discharge；Moreover, the fusing point of lithium is low, in the case of battery failure, easily with electrolysis
Matter, moisture, air vigorous reaction generate explosion；In addition, cathode of lithium in cyclic process, is also easy to produce dead zone, Li dendrite, influence
Cycle performance of battery or even Li dendrite can pierce through diaphragm, lead to internal short-circuit.
To avoid the effect negative using lithium anode bring lithium-sulfur cell, non-lithium an- ode has been obtained widely
Concern and research.Patent CN101465441 disclose it is a kind of using graphite as the preparation method of the lithium-sulfur cell of cathode and the battery,
It supplements lithium source (storing up lithium in advance) in sulphur anode in advance, cathode is steady using the structure without lithium source by the method for Electrochemical lithiation
Fixed graphite cathode improves safety and the cyclical stability of lithium-sulfur cell instead of the lithium metal of high activity.Patent
CN102694158A discloses a kind of preparation method of the lithium-sulfur cell of siliceous cathode of lithium with excess deposition lithium, which can drop
The formation probability of low Li dendrite improves cycle performance of battery and security performance.
There is the theoretical capacity higher than cathode of lithium containing silicium cathode, the theoretical capacity of silicium cathode is 4198mAh/g, aoxidizes sub- silicon
Theoretical capacity be 1964mAh/g, using containing silicium cathode substitution lithium anode prepare lithium-sulfur cell, lithium metal can be overcome
The generation of high chemical instability and Li dendrite, and safety and the cyclical stability of lithium-sulfur cell can be promoted.But
The preparation of such non-lithium metal battery needs to prepare pre- storage lithium electrode first, then dismantles battery, takes out pre- storage pole piece, so
Film-making again afterwards, is assembled into lithium-sulfur cell, such battery preparation method is more complex, and failure risk is big in preparation process, and prepares step
Rapid cumbersome condition harshness is unfavorable for industrial production, and more or less limits large-scale application.
Summary of the invention
It is an object of the present invention to provide a kind of in-situ preparation method of lithium-sulfur cell based on silicium cathode, the preparation method is controllable
Property it is high, simplify the preparation process flow of silicon substrate lithium-sulfur cell, evaded the failure risk of prior art, be easily converted into industrial life
Production technology.
The invention is realized in this way a kind of in-situ preparation method of the lithium-sulfur cell based on silicium cathode, comprising steps of
Step 1: preparing lithium/copper metal compound electric pole piece, which includes copper foil and is attached on copper foil as lithium
The lithium foil that the lithium metal in source is formed；
Step 2: according to positive pole plate of lithium-sulfur cell, lithium/copper metal compound electric pole piece, silicon-containing electrode piece and lithium/copper metal
The lamination sequence of compound electric pole piece carries out lamination, prepares three electrode lithium sulphur laminated batteries；
Step 3: the method for storing up lithium in advance using electrochemical in-situ carries out pre- storage lithium to silicon-containing electrode piece；
Step 4: in advance take out lithium/copper metal compound electric pole piece under gas shield environment after storage lithium, it is then right
Pole group degasification is simultaneously directly sealed, and the two electrode lithium-sulfur cells using silicon-containing electrode piece as cathode are obtained.
In the lithium/copper metal compound electric pole piece, the copper foil makes as the structural support of lithium metal, collector and tab
With；Or it is used as tab.
The copper foil is as the structural support of lithium metal, collector and tab in use, lithium foil/silicon-containing electrode piece capacity
Than for 1-10；The copper foil is as tab in use, lithium foil/silicon-containing electrode piece capacity ratio is 2-10.
The lithium foil with a thickness of 10-200 microns, copper foil with a thickness of 5-20 microns.
The silicon-containing electrode piece includes the silicon electrode piece that active material is elementary silicon and active material is the oxygen for aoxidizing sub- silicon
Change sub- silicon electrode piece.
In second step, when electrode lamination, the tab of positive pole plate of lithium-sulfur cell and silicon-containing electrode piece is made in battery the same side
For the first side of battery；Lithium/copper electrode piece tab side opposite in first side, the caudal as battery.
In third step, carrying out pre- storage lithium to silicon-containing electrode piece is with silicon-containing electrode piece for anode, with lithium/copper metal compound electric
Pole piece is cathode, stores up lithium in advance using electrochemical in-situ method.
Wherein, lithium is stored up using electrochemical in-situ method in advance, using the method for constant current discharge, discharge-rate 0.01C-
10C, blanking voltage are 0.2-0 volts；Or the method using constant voltage, discharge voltage are 0.2-0 volts, cut-off current is
0.001C-0.1C；Or the method for using constant current, constant voltage combined discharge, galvanostatic conditions, discharge-rate 0.01C-10C,
Blanking voltage is 0.2-0 volts, constant voltage condition, and discharge voltage is 0.2-0 volts, cut-off current 0.001C-0.1C.
In third step, the gas shield environment is nitrogen or argon gas protection environment.
In-situ preparation method provided by the invention based on the lithium-sulfur cell containing silicium cathode passes through three electrode lithium-sulfur cell bodies
The foundation of system carries out pre- storage lithium in situ, and this method, which eliminates, tears battery open, takes out pre- storage pole piece, lay equal stress on and replicate the mistake of standby pole piece
Journey overcomes and tears battery open, takes out pre- storage pole piece and lay equal stress on the failure risk during replicating standby pole piece, simplifies lithium-sulfur cell
Preparation flow, evaded process failure risk.The preparation method technique is simpler, and the production for being conducive to lithium-sulfur cell is promoted,
With great production practices meaning.
Detailed description of the invention
Fig. 1 is the pre- storage lithium curve of the embodiment of the present invention 1；
Fig. 2 is the schematic diagram of three electrode lithium-sulfur cells prepared by the embodiment of the present invention 1,3；
Fig. 3 is the schematic cross-section of three electrode lithium-sulfur cells prepared by the embodiment of the present invention 1,3；
Fig. 4 is the schematic cross-section of the two poles of the earth lithium-sulfur cell finally prepared in the embodiment of the present invention 1,2,3；
Fig. 5 is the pre- storage lithium curve of the embodiment of the present invention 2；
Fig. 6 is the pre- storage lithium curve of the embodiment of the present invention 3.
Specific embodiment
In the following, in conjunction with example, property feature and advantage is further described for the essence of the present invention, but the present invention not office
It is limited to listed embodiment.
Embodiment 1
A kind of in-situ preparation method based on the lithium-sulfur cell containing silicium cathode, in lithium/copper metal compound electric pole piece, copper foil is made
Come for the structural support of lithium metal, collector and tab using containing silicium cathode using pure silicon cathode, embodiment step is as follows:
(1) prepare that lithium/copper metal compound electric pole piece is stand-by, which is made of metallic lithium foil and copper foil first, by metal
Lithium foil is attached at the two sides of copper foil and reserves tab (other parts two sides of the copper foil in addition to tab is covered by metallic lithium foil), is made
The lithium/copper metal compound electric pole piece；
Wherein, lithium foil with a thickness of 40 microns, copper foil with a thickness of 8 microns, lithium foil/silicon-containing electrode piece capacity ratio is 3；
In addition, according to the preparation process flow of lithium-sulfur cell, prepare positive pole plate of lithium-sulfur cell, silicon-containing electrode piece, diaphragm,
Tab, battery case, electrolyte etc. are stand-by.
It should be noted that positive pole plate of lithium-sulfur cell, silicon-containing electrode piece, diaphragm, tab, battery case, electrolyte etc. are
Conventional material or customary preparation methods preparation.
(2) compound according to positive pole plate of lithium-sulfur cell, lithium/copper metal compound electric pole piece, silicon-containing electrode piece and lithium/copper metal
The lamination sequence of electrode slice carries out lamination, prepares three electrode lithium sulphur laminated batteries；
When electrode lamination, the tab of positive pole plate of lithium-sulfur cell and silicon-containing electrode piece is in battery the same side, as battery
First side, lithium/copper electrode piece tab side opposite in first side, the caudal as battery.
(3) method for storing up lithium in advance using electrochemical in-situ carries out pre- storage lithium, electrochemical pre-treatment, to contain to silicon-containing electrode
Silicon electrode piece is anode, is negative pole with lithium/copper compound electric pole piece, the side that can be combined using constant current discharge and constant voltage discharge
Formula, galvanostatic conditions, discharge-rate 0.1C, blanking voltage are 0.005 volt, and constant voltage condition, discharge voltage is 0.005 volt
Spy, cut-off current 0.02C.
(4) under argon gas dry environment, lithium/copper metal compound electric pole piece is taken out, then to pole group after storage lithium in advance
Degasification is simultaneously directly sealed, and the two electrode lithium-sulfur cells using silicon-containing electrode piece as cathode are obtained.
Embodiment 2
A kind of in-situ preparation method based on the lithium-sulfur cell containing silicium cathode, in lithium/copper metal compound electric pole piece, copper foil is made
Come for tab using containing silicium cathode using pure silicon cathode, embodiment step is as follows:
(1) prepare that lithium/copper metal compound electric pole piece is stand-by, which is made of metallic lithium foil and copper foil first, by metal
Lithium foil is mutually attached with the copper foil as tab, and the lithium/copper metal compound electric pole piece is made；
Wherein, lithium foil with a thickness of 200 microns, copper foil with a thickness of 8 microns, lithium foil/silicon-containing electrode piece capacity ratio is
5；
In addition, according to the preparation process flow of lithium-sulfur cell, prepare positive pole plate of lithium-sulfur cell, silicon-containing electrode piece, diaphragm,
Tab, battery case, electrolyte etc. are stand-by；
It should be noted that positive pole plate of lithium-sulfur cell, silicon-containing electrode piece, diaphragm, tab, battery case, electrolyte etc. are
Conventional material or customary preparation methods preparation.
(2) compound according to positive pole plate of lithium-sulfur cell, lithium/copper metal compound electric pole piece, silicon-containing electrode piece and lithium/copper metal
The lamination sequence of electrode slice carries out lamination, prepares three electrode lithium sulphur laminated batteries；
When electrode lamination, the tab of positive pole plate of lithium-sulfur cell and silicon-containing electrode piece is in battery the same side, as battery
First side, lithium/copper electrode piece tab side opposite in first side, the caudal as battery.
(3) method for storing up lithium in advance using electrochemical in-situ carries out pre- storage lithium, electrochemical pre-treatment, to contain to silicon-containing electrode
Silicon electrode piece is anode, is negative pole with lithium/copper compound electric pole piece, by the way of constant current discharge, galvanostatic conditions, and electric discharge times
Rate is 0.05C, and blanking voltage is 0.001 volt.
(4) under argon gas dry environment, lithium/copper metal compound electric pole piece is taken out, then to pole group after storage lithium in advance
Degasification is simultaneously directly sealed, and the two electrode lithium-sulfur cells using silicon-containing electrode piece as cathode are obtained.
Embodiment 3
A kind of in-situ preparation method based on the lithium-sulfur cell containing silicium cathode, in lithium/copper metal compound electric pole piece, copper foil is made
For the structural support of lithium metal, collector and tab come using, containing silicium cathode use containing 6% silicon materials graphite cathode, implement
Steps are as follows for example:
(1) prepare that lithium/copper metal compound electric pole piece is stand-by, which is made of metallic lithium foil and copper foil first, by metal
Lithium foil is attached at copper foil two sides and reserves tab (other parts two sides of the copper foil in addition to tab is covered by metallic lithium foil), and institute is made
State lithium/copper metal compound electric pole piece；
Wherein, lithium foil with a thickness of 40 microns, copper foil with a thickness of 8 microns, lithium foil/silicon-containing electrode piece capacity ratio is 3；
In addition, according to the preparation process flow of lithium-sulfur cell, prepare positive pole plate of lithium-sulfur cell, silicon-containing electrode piece, diaphragm,
Tab, battery case, electrolyte etc. are stand-by.
It should be noted that positive pole plate of lithium-sulfur cell, silicon-containing electrode piece, diaphragm, tab, battery case, electrolyte etc. are
Conventional material or customary preparation methods preparation.
(2) compound according to positive pole plate of lithium-sulfur cell, lithium/copper metal compound electric pole piece, silicon-containing electrode piece and lithium/copper metal
The lamination sequence of electrode slice carries out lamination, prepares three electrode lithium sulphur laminated batteries；
When electrode lamination, the tab of positive pole plate of lithium-sulfur cell and silicon-containing electrode piece is in battery the same side, as battery
First side, lithium/copper electrode piece tab side opposite in first side, the caudal as battery.
(3) method for storing up lithium in advance using electrochemical in-situ carries out pre- storage lithium, electrochemical pre-treatment, to contain to silicon-containing electrode
Silicon electrode piece is anode, is negative pole with lithium/copper compound electric pole piece, the side that can be combined using constant current discharge and constant voltage discharge
Formula, galvanostatic conditions, discharge-rate 0.1C, blanking voltage are 0.005 volt, and constant voltage condition, discharge voltage is 0.005 volt
Spy, cut-off current 0.02C.
(4) under argon gas dry environment, lithium/copper metal compound electric pole piece is taken out, then to pole group after storage lithium in advance
Degasification is simultaneously directly sealed, and the two electrode lithium-sulfur cells using silicon-containing electrode piece as cathode are obtained.
Fig. 2 shows the outline drawing of three electrode lithium-sulfur cells prepared by the embodiment of the present invention 1,3, including it is anode ear 1, siliceous
The silicium cathode tab 2 and lithium of electrode slice/copper metal compound electric pole piece tab 3.
Fig. 3 shows the sectional view of three electrode lithium-sulfur cells of the preparation of the embodiment of the present invention 1,3, includes lithium/copper metal
Compound electric pole piece 7, battery positive pole piece 6 and silicon-containing electrode piece 5, lithium/copper metal compound electric pole piece 7 is in battery positive pole piece 6
And between silicon-containing electrode piece 5, lithium/copper metal compound electric pole piece 7, battery positive pole piece 6 and silicon-containing electrode piece 5 and by diaphragm
4 separate carry out lamination.
It should be noted that if copper foil is only used as tab in use, situation in example 2, in Fig. 3
Lithium/copper metal compound electric pole piece 7 is to be replaced by lithium piece, and the sectional view of the three electrode lithium-sulfur cells prepared in embodiment 2 is other
Structure is as shown in Figure 2.
Fig. 4 shows the sectional view of the lithium-sulfur cell of the preparation of the embodiment of the present invention 1,2,3, including silicon-containing electrode piece
5, battery positive pole piece 6 and by the diaphragm 4 of silicon-containing electrode piece 5 and battery positive pole piece 6 being spaced apart.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of in-situ preparation method of the lithium-sulfur cell based on silicium cathode, which is characterized in that comprising steps of
Step 1: preparing lithium/copper metal compound electric pole piece, which includes copper foil and is attached on copper foil as lithium source
The lithium foil that lithium metal is formed；
Step 2: compound according to positive pole plate of lithium-sulfur cell, lithium/copper metal compound electric pole piece, silicon-containing electrode piece and lithium/copper metal
The lamination sequence of electrode slice carries out lamination, prepares three electrode lithium sulphur laminated batteries；
Step 3: the method for storing up lithium in advance using electrochemical in-situ carries out pre- storage lithium to silicon-containing electrode piece；
Step 4: lithium/copper metal compound electric pole piece is taken out under gas shield environment, after storage lithium then to pole group in advance
Degasification is simultaneously directly sealed, and the two electrode lithium-sulfur cells using silicon-containing electrode piece as cathode are obtained.
2. preparation method as described in claim 1, which is characterized in that in the lithium/copper metal compound electric pole piece, the copper foil
It is used as the structural support of lithium metal, collector and tab；Or it is used as tab.
3. preparation method as claimed in claim 2, which is characterized in that structural support of the copper foil as lithium metal, afflux
Body and tab are in use, lithium foil/silicon-containing electrode piece capacity ratio is 1-10；The copper foil as tab in use, lithium foil/it is siliceous
The capacity ratio of electrode slice is 2-10.
4. preparation method as described in claim 1, which is characterized in that the lithium foil with a thickness of 10-200 microns, the copper
Foil with a thickness of 5-20 microns.
5. preparation method as described in claim 1, which is characterized in that the silicon-containing electrode piece includes that active material is elementary silicon
Silicon electrode piece and active material be the oxidation Asia silicon electrode piece for aoxidizing sub- silicon.
6. preparation method as described in claim 1, which is characterized in that in second step, when electrode lamination, positive pole plate of lithium-sulfur cell
First side with the tab of silicon-containing electrode piece in battery the same side, as battery；Lithium/copper electrode piece tab first side it is opposite one
Side, the caudal as battery.
7. preparation method as described in claim 1, which is characterized in that in third step, to silicon-containing electrode piece carry out pre- storage lithium be with
Silicon-containing electrode piece is anode, be negative pole with lithium/copper metal compound electric pole piece, stores up lithium in advance using electrochemical in-situ method.
8. preparation method as claimed in claim 7, which is characterized in that lithium is stored up in advance using electrochemical in-situ method, using constant current
The method of electric discharge, or the method for using the method for constant voltage or using constant current, constant voltage combined discharge.
9. preparation method as described in claim 1, which is characterized in that in the 4th step, the gas shield environment is nitrogen or argon
Gas shielded environment.
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Effective date of registration: 20230208 Address after: 300457 No. 38, Haitai South Road, Binhai high tech Industrial Development Zone (outer ring), Binhai New Area, Tianjin Patentee after: TIANJIN LISHEN BATTERY JOINT-STOCK Co.,Ltd. Patentee after: Tianjin Juyuan New Energy Technology Co.,Ltd. Address before: 300384 Tianjin Xiqing District Binhai hi tech Industrial Development Zone (outer ring) 38 Haitai South Road Patentee before: TIANJIN LISHEN BATTERY JOINT-STOCK Co.,Ltd. |
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