CN109950465A - A kind of method of electrochemical stripping stratified material - Google Patents
A kind of method of electrochemical stripping stratified material Download PDFInfo
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- CN109950465A CN109950465A CN201910218078.3A CN201910218078A CN109950465A CN 109950465 A CN109950465 A CN 109950465A CN 201910218078 A CN201910218078 A CN 201910218078A CN 109950465 A CN109950465 A CN 109950465A
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- stratified material
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- 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 invention discloses a kind of methods of electrochemical stripping stratified material, and assembling first includes anode, diaphragm, electrolyte, the battery of the chief components such as cathode, by discharge process to stratified material progress intercalation；Secondly, the pole piece of intercalation is subjected to liquid ultrasonic removing, obtain the stratified material of single layer or few layer to the end, traditional lithium ion intercalation auxiliary liquid lift-off technology is replaced using the more abundant metallic element of resource reserve includes sodium, potassium, calcium, magnesium, aluminium or zinc, furthermore, it is bigger with respect to the stratified material interlamellar spacing of lithium ion intercalation after larger sized ion insertion since the size of other metal ions is bigger than lithium ion, so that intercalation stratified material can obtain better peeling effect.
Description
Technical field
The invention belongs to electrode material technical fields, and in particular to a kind of method of electrochemical stripping stratified material.
Background technique
Lithium ion battery has that energy density is high, energy efficiency is high, have extended cycle life, memory-less effect, repid discharge etc.
Advantage, thus have in the fields such as consumption electronic product and electric vehicle, peak load regulation network, accumulation power supply, aerospace huge
The market demand.For the challenge of reply the lithium ion battery performance, cost and the environment that face at present etc., development reserves are abundant,
Cheap and easy to get, electrochemical performance electrode material is current R&D direction.
Summary " the Ultrathin Two-Dimensional that hua zhang in 2015 is delivered on ACS NANO
Nanomaterials " it is discussed in detail and describes two-dimensional material: a kind of promising battery electrode material, and to two-dimensional material
Preparation method be classified arrangement.Two-dimensional material refers to that electronics only can be in the non-nanosize (1-100nm) of two dimensions
The material of upper free movement (plane motion), such as nano thin-film, superlattices and Quantum Well.Two-dimensional material is graceful along with 2004
Geim group, Chester university is successfully separated out graphite material-graphene (graphene) of monoatomic layer and proposes.Graphite
The unexpected physics of alkene, optical and electronic property, inspired researchers explore other have similar layer structure feature but
Two-dimension nano materials with multiple performance, such as hexagonal boron nitride (h-BN), transition metal dihalide (TMD), graphitic carbon nitrogen
Compound (g-C3N4), layered metal oxide and layered double-hydroxide (LDH).Many novel two dimensions are also explored in recent years
Crystal, as metal organic framework (MOF), covalent organic framework (COF), polymer, metal, black phosphorus (BP), siloxanes and
MXenes is greatly enriched the family of two-dimension nano materials.Two-dimension nano materials are because of its unique structure feature and outstanding
Performance, it has also become a kind of important materials of Condensed Matter Physics, material science and chemical field.In order to utilize its excellent performance,
People have developed a large amount of synthetic method, as mechanical cleavage, liquid removing, ion insertion and removing, anion exchange and removing,
Chemical vapor deposition (CVD) and wet chemistry synthesis etc..Importantly, before these two-dimension nano materials have a wide range of applications
Scape, such as electronics/photoelectron, catalysis, energy storage and conversion, biomedicine, sensor etc..
The preparation method of two-dimensional material has very much, there is mechanical stripping, the removing of mechanical-assisted liquid phase, ion insertion auxiliary stripping
From the removing of, ion exchange liquid phase and selective etch auxiliary liquid phase removing etc..Wherein ion insertion up-stripping is that comparison is classical
One kind.Its technical solution such as document (Angew.Chem., Int.Ed.2011,50,11093-11097) description, passes through building
Using lithium metal piece as cathode, molybdenum disulfide is the battery of anode, to reach intercalation purpose, then is assisted two with ultrasonic lift-off technology
Molybdenum sulfide removes the structure at two-dimensional nano piece.
Existing ion insertion up-stripping stratified material technology needs to use lithium metal, and lithium metal reserves are very limited,
Cause it is at high cost in use, meanwhile, lithium ion intercalation stripping effect is limited.The present invention using the sodium of rich reserves, potassium,
Calcium, magnesium, aluminium, zinc etc. carry out intercalation to stratified material, realize the removing to stratified material as to electrode, have significantly at
This advantage and the better peeling effect of acquisition.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of electrochemical stripping stratified material, and assembling includes anode first,
Diaphragm, electrolyte, the battery of the chief components such as cathode carry out intercalation to stratified material by discharge process；Secondly, will insert
The pole piece of layer carries out liquid ultrasonic removing, obtains the stratified material of single layer or few layer to the end, and metal used in this method is equal
Rich reserves, it is cheap, be easily obtained.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of method of electrochemical stripping stratified material, specifically includes the following steps:
Step 1: preparing cathode: under inert gas or anhydrous and oxygen-free environment, metal block is taken out from preservation vessel,
Straticulation is rolled, the sequin that diameter is 10-14mm is cut into, kerosene is added dropwise to soak protection；
Step 2: preparation anode: weighing stratified material, conductive agent and binder in proportion, solvent N-methyl pyrrole is added
Pyrrolidone is thoroughly mixed to form uniform sizing material, provides the plus plate current-collecting body of clean surface, slurry is then evenly applied to anode
Collection liquid surface forms anode active material layer, the disk of diameter 10mm is suppressed and cut into after being completely dried, obtains battery
Anode, it is spare；
Step 3: configuration electrolyte: weighing electrolytic salt and be added in nonaqueous solvents, dissolution is sufficiently stirred, is electrolysed
Liquid；
Step 4: preparing diaphragm: it is 16mm's that will insulate porous polymer film or inorganic porous film, which cut into diameter,
Disk after cleaning up, obtains diaphragm；
Step 5: assembled battery: under inert gas or anhydrous and oxygen-free environment, by the anode, diaphragm, cathode successively heap
Battery is folded or is wound into, electrolyte, which is added dropwise, makes diaphragm complete wetting, and above-mentioned stacking portion is then encapsulated into button shell, complete
At the assembling of battery；
Step 6: battery discharge: the battery assembled is installed into new prestige battery test system, set blanking voltage as
0.01-5V；After the completion of to be discharged, battery is removed, is stored in insulation vessel；
Step 7: tearing battery open: under inert gas or anhydrous and oxygen-free environment, again by the battery for end of discharging in step 6
Anode, diaphragm, cathode are splitted into, rinse pole piece is placed in naturally dry in inert gas or anhydrous and oxygen-free environment；
Step 8: transfer pole piece and ultrasound removing: in the positive plate transfer bottle that step 7 is dried, solvent is added, connects
Bottle is put into Ultrasound Instrument, power be 10-1000W under, it is 30-120 minutes ultrasonic.
Further, in step 1, the metal block is one of sodium block, potassium block, calcium block, MAG block, aluminium block, spelter.
Further, in step 2, the stratified material is molybdenum disulfide, two selenizing molybdenums, tungsten sulfide, one in tungsten selenide
Kind；
The conductive agent be conductive black, conductive carbon ball, electrically conductive graphite, carbon nanotube, conductive carbon fibre, graphene,
One of redox graphene is a variety of；
The binder is Kynoar, polytetrafluoroethylene (PTFE), polyvinyl alcohol, carboxymethyl cellulose, SBR rubber, gathers
One of olefines is a variety of；
Stratified material, conductive agent, binder mass ratio be 6.0-9.5:0.5-3.0:0.5-1.0.
Further, in step 2, the plus plate current-collecting body is aluminium, copper, iron, tin, zinc, nickel, titanium, any one in manganese
Or the alloy containing at least one above-mentioned metallic element, or the composite material containing at least one above-mentioned metallic element.
Further, in step 3, the electrolytic salt is hexafluorophosphate, tetrafluoroborate, chlorate, carbonate, sulphur
Hydrochlorate, nitrate, fluoride salt, fluoroform sulphonate, bis- (trifluoromethyl sulfonyl) inferior amine salts, double fluorine sulfimide salts, high chlorine
One of hydrochlorate is a variety of.
Further, in step 3, the nonaqueous solvents is organic solvent and ionic liquid, and the organic solvent is carbonic acid third
Enester, ethylene carbonate, diethyl carbonate, dimethyl carbonate, methyl ethyl carbonate, methyl formate, methyl acetate, N, N- dimethyl
Acetamide, fluorinated ethylene carbonate, methyl propionate, ethyl propionate, ethyl acetate, gamma-butyrolacton, tetrahydrofuran, 2- methyl four
Hydrogen furans, 1,3- dioxolanes, 4- methyl-1,3-dioxy pentamethylene, dimethoxymethane, 1,2- diformazan Ethylene Oxide, three second two
Diethylene glycol dimethyl ether, dimethyl sulfone, dimethyl ether, ethylene sulfite, sulfurous acid propylene rouge, two formicester of sulfurous acid, sulfurous acid diethyl rouge,
One of crown ether (12-crown-4) is a variety of；The ionic liquid is 1- ethyl-3-methylimidazole-hexafluorophosphate, 1- second
Base -3- methylimidazole-tetrafluoroborate, 1- ethyl-3-methylimidazole-bis trifluoromethyl sulfimide salt, 1- propyl -3- methyl
Imidazoles-hexafluorophosphate, 1- propyl -3- methylimidazole-tetrafluoroborate, 1- propyl -3- methylimidazole-bis trifluoromethyl sulphonyl
Inferior amine salt, 1- butyl -1- methylimidazole-hexafluorophosphate, 1- butyl -1- methylimidazole-tetrafluoroborate, 1- butyl -1- first
Base imidazoles-bis trifluoromethyl sulfimide salt, N- butyl-N- methylpyrrolidin- bis trifluoromethyl sulfimide salt, 1- butyl-
1- methylpyrrolidin- bis trifluoromethyl sulfimide salt, N- Methyl-N-propyl pyrrolidines-bis trifluoromethyl sulfimide salt, N-
First, propylpiperdine-bis trifluoromethyl sulfimide salt, N- first, one of butyl piperidine-bis trifluoromethyl sulfimide salt or
It is a variety of.
Further, in step 3, the concentration of electrolyte is 0.1-2mol/L.
Further, in step 4, the insulation porous polymer film or inorganic porous film be porous polypropylene film,
One of porous polyethylene film, porous compound polymer film, all-glass paper, porous ceramics diaphragm are a variety of.
Further, in step 8, the solvent is one of deionized water, dehydrated alcohol, isopropanol or a variety of.
Beneficial effects of the present invention:
A kind of method of electrochemical stripping stratified material provided by the invention uses the more abundant metal member of resource reserve
Plain (sodium, potassium, calcium, magnesium, aluminium, zinc) replaces traditional lithium ion intercalation auxiliary liquid lift-off technology, further, since other metals
The size of ion is bigger than lithium ion, after larger sized ion insertion more with respect to the stratified material interlamellar spacing of lithium ion intercalation
Greatly, so that intercalation stratified material can obtain better peeling effect.This method need first to prepare sodium ion, potassium ion, calcium from
Son, magnesium ion, aluminium ion, Zinc ion battery etc. realize effective intercalation to stratified material by discharge process, finally, dismantling electricity
Stratified material positive plate is taken out in pond, is placed in appropriate solvent and carries out ultrasonic removing, has apparent cost advantage and acquisition
Better peeling effect.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, will be described below to embodiment required
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is that embodiment 1 removes traversing of probe electron microscope observation figure, and wherein a is scanning electron microscope before removing
Observation chart；B is scanning electronic microscope observation figure after removing；
Fig. 2 is X ray diffracting spectrum before and after 1 intercalation of embodiment, and wherein a is X ray diffracting spectrum before intercalation；B is intercalation
X ray diffracting spectrum afterwards.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
It please refers to shown in Fig. 1-2, the present invention is a kind of method of electrochemical stripping stratified material, specifically includes following step
It is rapid:
It prepares the cathode of sode cell: in the glove box of inert gas shielding, sodium block being taken out from the kerosene of preservation,
Straticulation is rolled, and is cut into the sequin of 14mm with the tool of cutting, it is spare；
It prepares the anode of sode cell: 0.8g molybdenum disulfide, 0.1g conductive carbon black, 0.1g Kynoar is added to 2ml
In N-methyl pyrrolidone solution, it is fully ground acquisition uniform sizing material；Then slurry is evenly applied to copper foil surface (that is, just
Pole collector) and be dried in vacuo.The disk of diameter 10mm is cut into dry the electrode obtained piece, it is spare as anode after compacting；
Configuration electrolyte: it weighs 0.7023g sodium perchlorate and has been added to 3.2397g ethylene carbonate, 2.6201g carbonic acid two
The in the mixed solvent of methyl esters and 0.1425g fluorinated ethylene carbonate, stirring to ammonium perchlorate is completely dissolved, after stirring
It is spare as electrolyte；
It prepares diaphragm: being used as diaphragm spare after glass fiber membrane to be cut into the disk of diameter 16mm；
The assembling of sode cell: in the glove box of inert gas shielding, by the above-mentioned anode prepared, diaphragm, cathode according to
Secondary Close stack, electrolyte, which is added dropwise, makes diaphragm complete wetting, and above-mentioned stacking portion is then encapsulated into button shell, completes battery
Assembling；
Sode cell electric discharge: the battery assembled is installed into new prestige battery test system, set blanking voltage as
0.65V, it is to be discharged to remove after reaction, it is fitted into valve bag.
It tears battery open: in the glove box of inert gas shielding, the button cell encapsulated in valve bag being dismantled, take out two sulphur
Change molybdenum positive plate.Two drop dimethyl carbonate rinse pole pieces are added dropwise, is placed in glove box and waits naturally dry.
Ultrasound removing: the positive plate dried being taken out, is transferred in the bottle of 20mL, and the ethyl alcohol of 13mL or so is added.If
Determine ultrasonic power 110W, ultrasonic time 60min.
Embodiment 2-5
Ion insertion in embodiment 2-5 and embodiment 1 is identical as stripping process step, and difference is to select stratified material
It is different.
Embodiment 6-8
Ion insertion in embodiment 6-8 and embodiment 1 is identical as stripping process step, and difference is to select negative metal
Difference, while the electrolyte salt for corresponding to cathode also changes.
The form of battery of the present invention is not limited to button type, and plate, circle can also be designed to according to core component
The forms such as column type, laminated type.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention
Design or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (9)
1. a kind of method of electrochemical stripping stratified material, it is characterised in that: specifically includes the following steps:
Step 1: preparing cathode: under inert gas or anhydrous and oxygen-free environment, metal block being taken out from preservation vessel, is rolled into
Thin layer is cut into the sequin that diameter is 10-14mm, and kerosene is added dropwise to soak protection；
Step 2: preparation anode: weighing stratified material, conductive agent and binder in proportion, solvent N-methyl pyrrolidines is added
Ketone is thoroughly mixed to form uniform sizing material, provides the plus plate current-collecting body of clean surface, slurry is then evenly applied to anode collection
Body surface face forms anode active material layer, the disk of diameter 10mm is suppressed and cut into after being completely dried, is obtaining battery just
Pole, it is spare；
Step 3: configuration electrolyte: weighing electrolytic salt and be added in nonaqueous solvents, dissolution is sufficiently stirred, obtains electrolyte；
Step 4: preparing diaphragm: the disk that will insulate porous polymer film or inorganic porous film cut into diameter as 16mm,
After cleaning up, diaphragm is obtained；
Step 5: assembled battery: under inert gas or anhydrous and oxygen-free environment, the anode, diaphragm, cathode are stacked gradually or
It is wound into battery, electrolyte, which is added dropwise, makes diaphragm complete wetting, and above-mentioned stacking portion is then encapsulated into button shell, completes electricity
The assembling in pond；
Step 6: battery discharge: the battery assembled is installed into new prestige battery test system, set blanking voltage as
0.01-5V；After the completion of to be discharged, battery is removed, is stored in insulation vessel；
Step 7: tearing battery open: under inert gas or anhydrous and oxygen-free environment, the battery for end of discharging in step 6 being splitted into again
Anode, diaphragm, cathode, rinse pole piece are placed in naturally dry in inert gas or anhydrous and oxygen-free environment；
Step 8: transfer pole piece and ultrasound removing: in the positive plate transfer bottle that step 7 is dried, solvent is added, then will
Bottle is put into Ultrasound Instrument, 30-120 minutes ultrasonic in the case where power is 10-1000W.
2. a kind of method of electrochemical stripping stratified material according to claim 1, it is characterised in that: in step 1, institute
The metal block stated is one of sodium block, potassium block, calcium block, MAG block, aluminium block, spelter.
3. a kind of method of electrochemical stripping stratified material according to claim 1, it is characterised in that: in step 2, institute
The stratified material stated is one of molybdenum disulfide, two selenizing molybdenums, tungsten sulfide, tungsten selenide；
The conductive agent is conductive black, conductive carbon ball, electrically conductive graphite, carbon nanotube, conductive carbon fibre, graphene, reduction
One of graphene oxide is a variety of；
The binder is Kynoar, polytetrafluoroethylene (PTFE), polyvinyl alcohol, carboxymethyl cellulose, SBR rubber, polyolefin
One of class is a variety of；
Stratified material, conductive agent, binder mass ratio be 6.0-9.5:0.5-3.0:0.5-1.0.
4. a kind of method of electrochemical stripping stratified material according to claim 1, it is characterised in that: in step 2, institute
The plus plate current-collecting body stated be aluminium, copper, iron, tin, zinc, nickel, titanium, in manganese any one or containing at least one above-mentioned metallic element
Alloy, or the composite material containing at least one above-mentioned metallic element.
5. a kind of method of electrochemical stripping stratified material according to claim 1, it is characterised in that: in step 3, institute
Stating electrolytic salt is hexafluorophosphate, tetrafluoroborate, chlorate, carbonate, sulfate, nitrate, fluoride salt, trifluoro methylsulphur
One of hydrochlorate, bis- (trifluoromethyl sulfonyl) inferior amine salts, double fluorine sulfimide salts, perchlorate are a variety of.
6. a kind of method of electrochemical stripping stratified material according to claim 1, it is characterised in that: in step 3, institute
Stating nonaqueous solvents is organic solvent and ionic liquid, and the organic solvent is propene carbonate, ethylene carbonate, carbonic acid diethyl
Ester, dimethyl carbonate, methyl ethyl carbonate, methyl formate, methyl acetate, DMAC N,N' dimethyl acetamide, fluorinated ethylene carbonate, third
Sour methyl esters, ethyl propionate, ethyl acetate, gamma-butyrolacton, tetrahydrofuran, 2- methyltetrahydrofuran, 1,3- dioxolanes, 4-
Methyl-1,3-dioxy pentamethylene, dimethoxymethane, 1,2- diformazan Ethylene Oxide, triethylene glycol dimethyl ether, dimethyl sulfone, dimethyl ether,
One of ethylene sulfite, sulfurous acid propylene rouge, two formicester of sulfurous acid, sulfurous acid diethyl rouge, crown ether (12-crown-4) are more
Kind；The ionic liquid is 1- ethyl-3-methylimidazole-hexafluorophosphate, 1- ethyl-3-methylimidazole-tetrafluoroborate, 1-
Ethyl-3-methylimidazole-bis trifluoromethyl sulfimide salt, 1- propyl -3- methylimidazole-hexafluorophosphate, 1- propyl -3- first
Base imidazoles-tetrafluoroborate, 1- propyl -3- methylimidazole-bis trifluoromethyl sulfimide salt, 1- butyl -1- methylimidazole-six
Fluorophosphate, 1- butyl -1- methylimidazole-tetrafluoroborate, 1- butyl -1- methylimidazole-bis trifluoromethyl sulfimide salt,
N- butyl-N- methylpyrrolidin- bis trifluoromethyl sulfimide salt, 1- butyl -1- methylpyrrolidin- bis trifluoromethyl sulphonyl are sub-
Amine salt, N- Methyl-N-propyl pyrrolidines-bis trifluoromethyl sulfimide salt, N- first, propylpiperdine-bis trifluoromethyl sulphonyl are sub-
Amine salt, N- first, one of butyl piperidine-bis trifluoromethyl sulfimide salt or a variety of.
7. a kind of method of electrochemical stripping stratified material according to claim 1, it is characterised in that: in step 3, institute
The concentration of electrolyte stated is 0.1-2mol/L.
8. a kind of method of electrochemical stripping stratified material according to claim 1, it is characterised in that: in step 4, institute
State insulation porous polymer film or inorganic porous film be porous polypropylene film, it is porous polyethylene film, porous compound poly-
Close one of object film, all-glass paper, porous ceramics diaphragm or a variety of.
9. a kind of method of electrochemical stripping stratified material according to claim 1, it is characterised in that: in step 8, institute
Stating solvent is one of deionized water, dehydrated alcohol, isopropanol or a variety of.
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| CN110499636A (en) * | 2019-09-12 | 2019-11-26 | 航天材料及工艺研究所 | A kind of high thermal conductivity mesophase pitch-based carbon fibers intercalation stripping method |
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| CN114956178B (en) * | 2022-04-08 | 2023-08-08 | 湖南大学 | Electrochemical stripping method for two-dimensional layered material |
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