CN109802118A - A kind of preparation method of the rechargeable magnesium battery based on two selenizing vanadium anodes - Google Patents
A kind of preparation method of the rechargeable magnesium battery based on two selenizing vanadium anodes Download PDFInfo
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- CN109802118A CN109802118A CN201910060561.3A CN201910060561A CN109802118A CN 109802118 A CN109802118 A CN 109802118A CN 201910060561 A CN201910060561 A CN 201910060561A CN 109802118 A CN109802118 A CN 109802118A
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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 preparation methods of rechargeable magnesium battery based on two selenizing vanadium anodes, include the following steps: (1) by the widened VSe of interlamellar spacing2Nanometer sheet, acetylene black and gather inclined tetrafluoroethene and be added in N-Methyl pyrrolidone and stir pulp, is coated on carbon paper and electrode slice is made, and be dried in vacuo 18~25 hours in 50~80 DEG C, be then cut into sequin, obtain anode；(2) magnesium foil is then cut into small pieces with light is polishing to, obtains cathode；(3) anode obtained and cathode and glass fibre membrane and electrolyte are assembled into battery.Preparation method provided by the present invention based on two selenizing vanadium of rechargeable magnesium cell positive material is simple, by a step solvent-thermal method to VSe2Molecule interlayer is inserted into organic amine molecule in situ, obtains the VSe of interlamellar spacing increase2Nanometer sheet, conducive to the transmission of magnesium ion.
Description
Technical field
This application involves electrochemical material technical fields, in particular to a kind of filling based on two selenizing vanadium anodes
The preparation method of electric magnesium cell.
Background technique
It is today that exhausted and environmental pollution increasingly sharpens in the energy, countries in the world are all utilizing the energy energetically, saving
The limited energy.In recent years, many researchers are dedicated to exploring exploitation new energy memory device to solve high efficiency of energy benefit
Use problem.Lithium ion battery has extended cycle life since with energy density height, power density is big and memory-less effect etc. is excellent
Point is widely used in peak value storage of various mancarried electronic aids, electric car and smart grid etc..
Cause lithium ion battery at high cost however, the content of elemental lithium in nature is considerably less, while lithium ion battery
In sharp Li dendrite easy to form, Li dendrite can puncture diaphragm, make battery short circuit, cause safety problem.These problems make
The large-scale application of lithium ion battery is restricted.
Recently, rechargeable magnesium battery receives the great research interest of researchers.Compared with lithium ion battery, magnesium cell
With many advantages: the reserves of magnesium in nature are very rich, and environmental sound；Magnesium have lower reduction potential (-
2.37V vs.RHE)；The theoretical volumetric capacity of magnesium cell is up to 3383mAh cm-3, it is nearly twice of lithium ion battery；Magnesium from
Sub- gan, which is moved, carries two charges, so that magnesium cell has bigger energy density；Magnesium ion is not easy to be formed dendrite, safety compared with
It is high.Therefore, magnesium cell has very big potentiality in extensive electrochemical energy storage device.
But the development of magnesium cell at present, mainly by both sides obstacle, one is a lack of anodic stabilization with higher
Property and the electrolyte compatible with positive and negative anodes；Second is that being easy since the lesser divalent magnesium ion of radius has stronger polarization
Coulomb effect occurs with the lattice anion of positive electrode, magnesium ion is caused to be difficult the intercalation/deintercalation in positive electrode, therefore,
High capacity is found, macrocyclic positive electrode seems extremely important.
2000, Aubach et al. successfully assembled magnesium cell for the first time, and positive electrode used has Chevrel phase
Mo6S8.Electrolyte used is 0.25M Mg (AlCl2BuEt)2Tetrahydrofuran solution.Then, a variety of materials are all used for magnesium electricity
Pond anode is studied, including transient metal sulfide, transition metal oxide, polyanionic material, organic polymer etc..But
It is that most of magnesium cell anode materials all suffer from that operating voltage is lower, and discharge capacity is low, high rate performance difference and cyclical stability
Poor problem.Therefore, the excellent positive electrode of design performance is extremely important to the development and application of magnesium cell.
Summary of the invention
In the prior art, there is no the researchs that two selenizing vanadium are used for magnesium cell system to report.Therefore, the invention
Ground provides a kind of macrocyclic rechargeable magnesium battery of high capacity based on two selenizing vanadium anodes.
Since divalent magnesium ion has polarization more stronger than lithium ion and sodium ion, we are biggish by interlamellar spacing
VSe2For rechargeable magnesium battery, due to divalent magnesium ion and VSe2The electrostatic interaction of lattice anion is weaker, be conducive to magnesium from
The intercalation/deintercalation of son, therefore show excellent battery performance.
The preparation method of the rechargeable magnesium battery, includes the following steps:
(1) by the widened VSe of interlamellar spacing2Nanometer sheet, acetylene black and gathers inclined tetrafluoroethene and be added in N-Methyl pyrrolidone
Pulp is stirred, is coated on carbon paper and electrode slice is made, and is dried in vacuo 18~25 hours in 50~80 DEG C, roundlet is then cut into
Piece obtains anode；
(2) magnesium foil is then cut into small pieces with light is polishing to, obtains cathode；
(3) anode obtained and cathode and glass fibre membrane and electrolyte are assembled into battery.
Further, in the step 1 of the above method, preferably 60 DEG C are dried in vacuo 24 hours.
Specifically, the widened VSe of the interlamellar spacing2Nanometer sheet, acetylene black gather the mass ratio of inclined tetrafluoroethene for 8:1:
1~6:3:1.Preferred proportion: 8:1:1.
Specifically, the dosage of the N-Methyl pyrrolidone is 1.0g VSe2Use 4~5mLN- methyl pyrrolidone.
Specifically, the widened VSe of the interlamellar spacing2Nanometer sheet obtains by the following method:
(1) vanadium source and selenium source are proportionally added into Amine Solutions, stir half an hour；
(2) mixed solution in (1) is transferred in reaction kettle, is reacted 16~24 hours at 160~200 DEG C；
(3) it after natural cooling, is centrifuged, washing is dried in vacuo up to the widened VSe of interlamellar spacing2Nanometer sheet.
Further, it in the step 2 of the above method, is reacted 24 hours preferably at 180 DEG C.
Specifically, the ratio of the vanadium source and selenium source is molar ratio 1:5~1:2.5.Preferred molar ratio 1:5.
Specifically, the dosage of the Amine Solutions is 20~50mL.
Specifically, the vanadium source is ammonium metavanadate, vanadyl acetylacetonate, sodium metavanadate, sodium orthovanadate.
Specifically, the selenium source is sodium selenite, selenium dioxide, selenium powder, selenous acid.
Specifically, the organic amine is n-octyl amine, 2 ethyl hexylamine, 3- ethyl -3- hexylamine, diethylenetriamines.
Specifically, the electrolyte is the tetrahydrofuran solution of bis- (two silicon nitrine of hexamethyl) magnesium/magnesium dichloride-based.
The utility model has the advantages that the preparation method letter provided by the present invention based on two selenizing vanadium of rechargeable magnesium cell positive material
It is single, by a step solvent-thermal method to VSe2Molecule interlayer is inserted into organic amine molecule in situ, obtains the VSe of interlamellar spacing increase2Nanometer
Piece, conducive to the transmission of magnesium ion.Using magnesium cell made from this method, discharge capacity with higher, and have excellent
High rate performance and long circulating stability, performance are better than most of magnesium cell systems reported at present.
Detailed description of the invention
Fig. 1 is VSe2The SEM picture of nanometer sheet.
Fig. 2 magnesium cell assembling schematic diagram.
Fig. 3 is battery performance test result schematic diagram under different current densities.
Fig. 4 is the long circulating test chart of battery under 500mA g-1 current density.
Specific embodiment
In order to make those skilled in the art more fully understand application scheme, below in conjunction in the embodiment of the present application
Attached drawing, the technical scheme in the embodiment of the application is clearly and completely described, it is clear that described embodiment is only
The embodiment of the application a part, instead of all the embodiments.
Embodiment 1
The widened VSe of interlamellar spacing2The preparation method of nanometer sheet:
(1) a certain amount of octylame solution is added in the amount of ammonium metavanadate and sodium selenite 1:5 in molar ratio, stirring half is small
When；
(2) gained mixed solution is transferred in the reaction kettle of polytetrafluoro, is reacted 24 hours at 180 DEG C；
(3) it after natural cooling, is centrifuged, washing is dried in vacuo up to the widened VSe of interlamellar spacing2Nanometer sheet.
As shown in Figure 1, the VSe2At flaky nanometer structure.
Embodiment 2
The preparation of battery:
(1) by the widened VSe of interlamellar spacing2Nanometer sheet, acetylene black gather inclined tetrafluoroethene with mass ratio for 8:1:1~6:3:1
It is ground uniformly in mortar, suitable N-Methyl pyrrolidone is then added, stirs into homogenate；
(2) above-mentioned homogenate is evenly coated on carbon paper, it is dry under vacuum, it is then cut into the disk that diameter is 1.4 centimetres,
It is i.e. positive, it is then transferred into the glove box full of Ar；
(3) magnesium sheet is polishing to light with carborundum paper in glove box, it is then natural with tetrahydrofuran wiped clean
It dries, is cut into the disk that diameter is 1.2 centimetres, i.e. cathode；The molybdenum sheet of 0.05mm thickness is cut into the circle that diameter is 2.0 centimetres simultaneously
Piece, for protecting motor casing；
(4) battery assembles: upward, the molybdenum sheet sheared is put into for anode cover, is put into positive plate (upward), is put into diaphragm, drop
Enter appropriate electrolyte, be put into magnesium sheet cathode, be put into gasket and elastic slice, finally buckle negative electrode casing, it is carried out with battery sealing machine
It encapsulates (Fig. 2)；
(5) battery standing 12~24 hours, setup test.
Embodiment 3
Electrochemical property test:
The magnesium cell is assembled in the argon gas glove box of anhydrous and oxygen-free, and electrochemical property test is in blue electrical testing system
It is completed in system (LAND).Specific step is as follows:
Glove box is opened, by VSe2It is button-shaped that anode, magnesium foil cathode, glass fibre membrane and electrolyte are assembled into CR2032
Battery.
Blue electrical measurement test system is opened, experiment parameter, starting test are set.
The VSe2When nanometer sheet is magnesium cell anode, there is good chemical property.Fig. 3 a and b are shown with VSe2Nanometer
Piece is the charging and discharging curve and high rate performance for being in different current densities as the magnesium cell of anode, it can be seen that in 500mA
g-1High current density under, discharge capacity of the cell is still up to 91mAh g-1, this high rate performance is most of also superior to what is reported at present
Work.As shown in figure 4, the battery is in 500mA g-1High current density under, first circle discharge capacity is up to 190mAh g-1, circulation
After 800 circles, capacity still has 55mAh g-1.The performance of the magnesium cell is got well than the magnesium cell performance of current most of reports, right
The development tool of magnesium cell has very important significance.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application.
Claims (10)
1. a kind of preparation method of the rechargeable magnesium battery based on two selenizing vanadium anodes, which comprises the steps of:
(1) by the widened VSe of interlamellar spacing2Nanometer sheet, acetylene black and gathers inclined tetrafluoroethene and be added in N-Methyl pyrrolidone and stir into
Pulpous state is coated on carbon paper and electrode slice is made, and is dried in vacuo 18~25 hours in 50~80 DEG C, is then cut into sequin, obtains
Anode；
(2) magnesium foil is then cut into small pieces with light is polishing to, obtains cathode；
(3) anode obtained and cathode and glass fibre membrane and electrolyte are assembled into battery.
2. the preparation method of the rechargeable magnesium battery according to claim 1 based on two selenizing vanadium anodes, which is characterized in that
The widened VSe of the interlamellar spacing2Nanometer sheet, acetylene black gather the mass ratio of inclined tetrafluoroethene for 8:1:1~6:3:1.
3. the preparation method of the rechargeable magnesium battery according to claim 1 based on two selenizing vanadium anodes, which is characterized in that
The dosage of the N-Methyl pyrrolidone is 1.0g VSe2Use 4~5mLN- methyl pyrrolidone.
4. the preparation method of the rechargeable magnesium battery according to claim 1 based on two selenizing vanadium anodes, which is characterized in that
The widened VSe of the interlamellar spacing2Nanometer sheet obtains by the following method:
(1) vanadium source and selenium source are proportionally added into Amine Solutions, stir half an hour；
(2) mixed solution in (1) is transferred in reaction kettle, is reacted 16~24 hours at 160~200 DEG C；
(3) it after natural cooling, is centrifuged, washing is dried in vacuo up to the widened VSe of interlamellar spacing2Nanometer sheet.
5. the preparation method of the rechargeable magnesium battery according to claim 4 based on two selenizing vanadium anodes, which is characterized in that
The ratio of the vanadium source and selenium source is molar ratio 1:5~1:2.5.
6. the preparation method of the rechargeable magnesium battery according to claim 1 based on two selenizing vanadium anodes, which is characterized in that
The dosage of the Amine Solutions is 20~50mL.
7. the preparation method of the rechargeable magnesium battery according to claim 1 based on two selenizing vanadium anodes, which is characterized in that
The vanadium source is ammonium metavanadate, vanadyl acetylacetonate, sodium metavanadate, sodium orthovanadate.
8. the preparation method of the rechargeable magnesium battery according to claim 1 based on two selenizing vanadium anodes, which is characterized in that
The selenium source is sodium selenite, selenium dioxide, selenium powder, selenous acid.
9. the preparation method of the rechargeable magnesium battery according to claim 1 based on two selenizing vanadium anodes, which is characterized in that
The organic amine is n-octyl amine, 2 ethyl hexylamine, 3- ethyl -3- hexylamine, diethylenetriamines.
10. the preparation method of the rechargeable magnesium battery according to claim 1 based on two selenizing vanadium anodes, feature exist
In the tetrahydrofuran solution that, the electrolyte is bis- (two silicon nitrine of hexamethyl) magnesium/magnesium dichloride-based.
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Cited By (9)
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|---|---|---|---|---|
| CN110556509A (en) * | 2019-08-14 | 2019-12-10 | 南京大学 | Method for performing surface protection and passivation treatment on metallic lithium cathode by using fluorine-containing organic matter, product and application |
| CN112490440A (en) * | 2020-12-07 | 2021-03-12 | 郑州轻工业大学 | Liquid phase reaction prepared oxyselenide/sulfoselenide, method and application thereof |
| CN112952060A (en) * | 2021-02-26 | 2021-06-11 | 广东工业大学 | Vanadium diselenide/carbon cellulose composite material and preparation method and application thereof |
| CN113929072A (en) * | 2021-10-14 | 2022-01-14 | 深圳大学 | LFP @ VSe2 composite positive electrode material and preparation method thereof |
| CN114314528A (en) * | 2021-12-20 | 2022-04-12 | 深圳大学 | Two-dimensional layered nanosheet and preparation method and application thereof |
| CN114724866A (en) * | 2022-03-11 | 2022-07-08 | 上海健康医学院 | Binder-free vanadium-doped nickel selenide nano array material and preparation method and application thereof |
| CN114899363A (en) * | 2022-05-11 | 2022-08-12 | 中国矿业大学 | Conductive polymer column support VS 2 Magnesium secondary battery positive electrode material and preparation method thereof |
| CN114920207A (en) * | 2022-05-05 | 2022-08-19 | 哈尔滨工业大学 | Flower-shaped VSe 2 Method for synthesizing nano material |
| CN115036504A (en) * | 2022-07-22 | 2022-09-09 | 济南易航新材料科技有限公司 | Flower-like vanadium diselenide @ carbon fiber nano material, preparation method and application thereof, and magnesium-lithium double-ion battery |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110556509A (en) * | 2019-08-14 | 2019-12-10 | 南京大学 | Method for performing surface protection and passivation treatment on metallic lithium cathode by using fluorine-containing organic matter, product and application |
| CN112490440A (en) * | 2020-12-07 | 2021-03-12 | 郑州轻工业大学 | Liquid phase reaction prepared oxyselenide/sulfoselenide, method and application thereof |
| CN112952060A (en) * | 2021-02-26 | 2021-06-11 | 广东工业大学 | Vanadium diselenide/carbon cellulose composite material and preparation method and application thereof |
| CN112952060B (en) * | 2021-02-26 | 2022-08-19 | 广东工业大学 | Vanadium diselenide/carbon cellulose composite material and preparation method and application thereof |
| CN113929072A (en) * | 2021-10-14 | 2022-01-14 | 深圳大学 | LFP @ VSe2 composite positive electrode material and preparation method thereof |
| CN114314528A (en) * | 2021-12-20 | 2022-04-12 | 深圳大学 | Two-dimensional layered nanosheet and preparation method and application thereof |
| CN114724866A (en) * | 2022-03-11 | 2022-07-08 | 上海健康医学院 | Binder-free vanadium-doped nickel selenide nano array material and preparation method and application thereof |
| CN114920207A (en) * | 2022-05-05 | 2022-08-19 | 哈尔滨工业大学 | Flower-shaped VSe 2 Method for synthesizing nano material |
| CN114920207B (en) * | 2022-05-05 | 2024-02-09 | 哈尔滨工业大学 | Flower-shaped VSe 2 Method for synthesizing nano material |
| CN114899363A (en) * | 2022-05-11 | 2022-08-12 | 中国矿业大学 | Conductive polymer column support VS 2 Magnesium secondary battery positive electrode material and preparation method thereof |
| CN114899363B (en) * | 2022-05-11 | 2023-11-21 | 中国矿业大学 | Conductive polymer column support VS 2 Magnesium secondary battery anode material and preparation method thereof |
| CN115036504A (en) * | 2022-07-22 | 2022-09-09 | 济南易航新材料科技有限公司 | Flower-like vanadium diselenide @ carbon fiber nano material, preparation method and application thereof, and magnesium-lithium double-ion battery |
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Application publication date: 20190524 |