CN104091925B - Multiple edge MoS2nanometer sheet/Graphene electrochemistry storage magnesium combination electrode and preparation method - Google Patents
Multiple edge MoS2nanometer sheet/Graphene electrochemistry storage magnesium combination electrode and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of multiple edge MoS2/ Graphene electrochemistry storage magnesium combination electrode and preparation method thereof, its electrochemistry storage magnesium active substance is the multiple edge MoS of few number of plies2Nanometer sheet and the composite nano materials of Graphene, MoS in composite nano materials2Being 1:2 with the ratio of the amount of the material of Graphene, its component and mass percentage content thereof be: multiple edge MoS2Nanometer sheet/graphite composite nano materials is 80%, acetylene black 10%, carboxymethyl cellulose 5%, Kynoar 5%.Preparation process: first prepare the multiple edge MoS of few number of plies2Nanometer sheet/graphene composite nano material, by prepared composite nano materials and acetylene black and the uniform slurry of Kynoar furnishing, is coated onto on the foam copper of collector equably using this slurry, and dried rolling obtains electrochemistry storage magnesium combination electrode.Electrochemistry storage magnesium combination electrode prepared by the present invention has high electrochemistry storage magnesium capacity.
Description
Technical field
The present invention relates to electrochemistry storage magnesium electrode and preparation method thereof, particularly relate to a kind of multiple edge MoS2/ Graphene electrochemistry storage magnesium combination electrode and preparation method thereof, belongs to new energy materials, energy storage and switch technology field.
Background technology
Along with modern mobile communication, new-energy automobile and the development of intelligent grid, novel electrochmical power source serves the most important effect in modern society.Traditional secondary cell, if lead-acid accumulator is owing to it is containing harmful metallic element Pb, its application is restricted.Lithium ion battery has the excellent properties such as high specific energy, memory-less effect, environmental friendliness, is widely used in the Portable movable electrical equipment such as mobile phone and notebook computer.As electrokinetic cell, lithium ion battery is also with a wide range of applications at aspects such as electric bicycle, electric automobile and intelligent grids.But limited due to the safety never solution the most carefully of lithium ion battery and lithium resource, lithium ion battery still there is also a lot of work as the extensive application of electrokinetic cell and storage battery and to do.Along with the development of new-energy automobile and the large-scale application of storage battery are in the urgent need to finding a kind of a kind of cheap, environmental friendliness that can substitute existing secondary cell system and the secondary cell of height ratio capacity.Owing to divalent magnesium ion has less radius, can be with electrochemical intercalation and deintercalation in the compound of some Rotating fields, such as: inorganic transition metal oxide, sulfide etc..Additionally magnesium also have aboundresources, cheap, specific energy is high, nontoxic and process the advantages such as convenient.Therefore, rechargeable magnesium ion battery the most also becomes the research system of a new secondary cell.But up to the present the electrode material as high performance electrochemistry storage magnesium is the most little.
MoS2Have with graphite-like as layer structure, be the S-Mo-S that combines of the strongest covalent bond in its layer, be the most then more weak Van der Waals force.MoS2More weak interlaminar action power and bigger interlamellar spacing allow to introduce external atom or molecule by insertion reaction at its interlayer.Such characteristic makes MoS2Material can be as the material of main part of insertion reaction.Therefore, MoS2It it is the electrode material of a kind of rising electrochemistry storage magnesium.Li etc. are prepared for nano level MoS by hydro-thermal reaction approach2 ,Have studied its electrochemistry storage magnesium performance, but its electrochemistry storage magnesium capacity is relatively low, only 50-80 mAh/g (X. L. Li, Y.
D. Li, J. Phys. Chem. B, 2004,108:13893).
Two-dimension nano materials has the characteristic of numerous excellence with the pattern of its uniqueness, and its research causes the great interest of people.Graphene is most typical two-dimension nano materials, and the two-dimensional nano chip architecture of its uniqueness makes the performances such as the physics of its numerous uniquenesses, chemistry and mechanics, has important scientific research meaning and technology application prospect widely.Graphene has high specific surface area, high conduction and heat conductivility, high charge mobility, excellent mechanical property, the characteristic of these excellences makes Graphene be with a wide range of applications in fields such as nano electron device, novel catalyst material and electrochemistry energy storage and energy conversion.
The immense success that the discovery of Graphene and research thereof obtain excites the great interest that other inorganic two-dimension nano materials are studied by people, such as monolayer or the transition metal dichalcogenide etc. of few number of plies.Recently, Graphene concept has expanded to the inorganic compound of other layer structures from material with carbon element, namely for the inorganic material of layer structure, when its number of plies reduces (less than about 7 layers), when being especially reduced to monolayer, its electronic property or band structure can produce significantly change, thus cause which show the physics different from corresponding body phase material and chemical characteristic.In addition to Graphene, when body phase MoS2It is reduced to few number of plies (especially during monolayer), it is shown that Wuli-Shili-Renli system approach visibly different with body phase material.Research shows monolayer or the MoS of few number of plies2Nanometer sheet has more preferable electrochemistry storage magnesium performance.But as the electrode material of electrochemistry storage magnesium, MoS2The lowest electric conductivity have impact on its application performance.
Due to MoS2Nanometer sheet has similar two-dimensional nano sheet pattern with Graphene, and both have good similarity on microscopic appearance and crystal structure.If by MoS2Nanometer sheet and Graphene are combined the composite of preparation, the high conduction performance of graphene nanometer sheet can improve the electric conductivity of composite further, strengthen the electron transmission in electrochemistry storage magnesium electrode course of reaction, the electrochemistry storage magnesium performance of composite can be improved further.With common MoS2Nanometer sheet compares, few number of plies multiple edge MoS2Nanometer sheet can provide the shortest magnesium ion diffusion admittance, has more contact area with electrolyte.Therefore, multiple edge MoS2The composite nano materials of nanometer sheet/Graphene has more preferable electrochemistry storage magnesium performance.
But, up to the present, use multiple edge MoS2Nanometer sheet/graphene composite nano material have not been reported as electrochemistry storage magnesium combination electrode and the preparation thereof of electroactive substance.First the present invention is raw material with graphene oxide and sodium molybdate, by adding hydrothermal method and the heat treatment subsequently of ionic liquid, is prepared for multiple edge MoS2The composite nano materials of nanometer sheet/Graphene, then uses multiple edge MoS2The composite nano materials of nanometer sheet/Graphene, as the active substance of electrochemistry storage magnesium, is prepared for the combination electrode of electrochemistry storage magnesium.The present invention prepares multiple edge MoS2The method of/Graphene electrochemistry storage magnesium combination electrode has simple, convenient and is easily enlarged industrial applications a little.
Summary of the invention
It is an object of the invention to provide a kind of multiple edge MoS2/ Graphene electrochemistry storage magnesium combination electrode and preparation method thereof, the multiple edge MoS that electrochemistry storage magnesium active substance is few number of plies of described combination electrode2The composite nano materials of nanometer sheet/Graphene, multiple edge MoS in composite nano materials2The ratio of the amount of the material of nanometer sheet and Graphene is 1:2, and the component of combination electrode and mass percentage content thereof be: multiple edge MoS2Nanometer sheet/graphene composite nano material 80%, acetylene black 10%, carboxymethyl cellulose 5%, Kynoar 5%.
In technique scheme, few number of plies refers to 6 layers or less than 6 layers.
As preferably, multiple edge MoS2The number of plies of nanometer sheet is 3-6 layer.
Multiple edge MoS of the present invention2The preparation method of/Graphene electrochemistry storage magnesium combination electrode is carried out in the steps below:
(1) by graphene oxide ultrasonic disperse in deionized water, ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate ([BMIM] BF is added4), its structure is shown in the schematic diagram of Fig. 1, and be sufficiently stirred for, then Cys and sodium molybdate are sequentially added, and be stirred continuously and make Cys and sodium molybdate be completely dissolved, the ratio of the amount of the material of Cys and sodium molybdate consumption is 5:1, and the ratio of sodium molybdate and the amount of the material of graphene oxide is at 1:2；
(2) mixed dispersion that step (1) obtains is transferred in hydrothermal reaction kettle, and add deionized water adjustment volume to the 80% of hydrothermal reaction kettle nominal volume, the content of ionic liquid is 5 mL/L, this reactor is put in constant temperature oven, at 240 DEG C after hydro-thermal reaction 24 h, it is allowed to naturally cool to room temperature, hydro-thermal solid product is collected with centrifugation, and fully wash with deionized water, it is vacuum dried at 100 DEG C, obtained by hydro-thermal solid product in nitrogen/hydrogen mixed gas atmosphere at 500 DEG C heat treatment 2 h, in mixed gas, the volume fraction of hydrogen is 10%, prepare multiple edge MoS2The composite nano materials of nanometer sheet/Graphene；
(3) by the multiple edge MoS of above-mentioned preparation2Nanometer sheet/graphene composite nano material stores magnesium active substance as the electrochemistry of electrode, with acetylene black, the N-Methyl pyrrolidone solution of the Kynoar of carboxymethyl cellulose and mass fraction 5% is under agitation sufficiently mixed the uniform slurry of furnishing, each component and mass percentage content: multiple edge MoS2Nanometer sheet/graphene composite nano material 80%, acetylene black 10%, carboxymethyl cellulose 5%, Kynoar 5%, this slurry is coated onto equably on the foam copper of collector, is dried, after rolling, obtains multiple edge MoS2/ Graphene electrochemistry storage magnesium combination electrode.
Above-mentioned graphene oxide uses the Hummers method improved to prepare.
The multiple edge MoS of the present invention2/ Graphene electrochemistry storage magnesium combination electrode and preparation method thereof has the advantage that
Surface of graphene oxide and edge with a lot of oxygen-containing functional groups (such as hydroxyl, carbonyl, carboxyl), these oxygen-containing functional groups make graphene oxide more easily be dispersed in water or organic liquid, but these oxygen-containing functional groups make surface of graphene oxide with negative charge so that graphene oxide and the MoO with negative charge4 2-Ion is incompatible, and the present invention is piled up by Π-Π and the positively charged ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate schematic diagram of Fig. 1 (its structure see) is first adsorbed onto surface of graphene oxide, MoO by electrostatic interaction4 2-Ion is just easier to interact with the graphene oxide having adsorbed ionic liquid combine.Research shows MoS2The surface energy of its basic side, therefore, MoS prepared by general hydro-thermal reaction can be much higher than in the surface at nanometer sheet edge2Nanometer sheet edge is less.Prepare the MoS of more multiple edge2Nanometer sheet will manage to reduce MoS2The surface energy at nanometer sheet edge.In hydro-thermal reaction, add ionic liquid, MoS can be reduced2The surface energy at nanometer sheet edge, the hydro-thermal reaction approach therefore assisted by ionic liquid can prepare the MoS of more multiple edge2The composite nano materials of nanometer sheet/Graphene.Compared with common quaternary cationics, the positive charge of ionic liquid cationic be distributed across in nitrogen heterocyclic ring (such as: imidazole ring, see Fig. 1), this nitrogen heterocyclic ring containing positive charge can preferably interact with electronegative graphene oxide than general quaternary cationics.This is because positively charged quaternary ammonium N is sp in general quaternary cationics3Hydridization, in succession 3 methyl and a long alkyl chain, hamper the direct electrostatic attraction effect of quaternary ammonium N and graphene oxide；And the N in heterocycle is the sp of planar structure in ionic liquid2Hydridization, is piled up by Π-Π and electrostatic attraction can preferably interact with graphene oxide.Composite prepared by the present invention has accurate three-dimensional loose structure, MoS therein2It is the nanometer sheet of few number of plies multiple edge, it is provided that the shortest magnesium ion diffusion admittance, increases the contact area with electrolyte, contribute to being obviously enhanced its electrochemistry storage magnesium performance.Therefore, the multiple edge MoS of the present invention2/ Graphene electrochemistry storage magnesium combination electrode has the electrochemistry storage magnesium performance being obviously enhanced.The preparation method of the present invention also has feature that is simple, convenient and that be easily enlarged industrial applications.
Accompanying drawing explanation
Fig. 1 ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate ([BMIM] BF4) structural representation.
The multiple edge MoS that Fig. 2 embodiment 1 prepares2The XRD figure of nanometer sheet/graphene composite nano material.
The multiple edge MoS that Fig. 3 embodiment 1 prepares2The SEM shape appearance figure of nanometer sheet/graphene composite nano material and transmission electron microscope photo.
MoS prepared by Fig. 4 comparative example2The XRD figure of nanometer sheet/graphene composite nano material.
MoS prepared by Fig. 5 comparative example2TEM, HRTEM photo of nanometer sheet/graphene composite nano material.
Detailed description of the invention
The present invention is further illustrated below in conjunction with embodiment.
Graphene oxide in following example uses the Hummers method improved to prepare: 0oUnder C ice bath, by 10.0 mmol (0.12 g) graphite powder dispersed with stirring to 50 mL concentrated sulphuric acids, it is stirred continuously down and is slowly added into KMnO4, added KMnO4Quality be 4 times of graphite powder, stir 50 minutes, when temperature rises to 35 DEG C, be slowly added into 50 mL deionized waters, be stirred for 30 minutes, add the H of 15 mL mass fractions 30%2O2, stir 30 minutes, through centrifugation, after mass fraction 5%HCl solution, deionized water and acetone cyclic washing, obtain graphene oxide successively.
Embodiment 1.
1) by 2.5 mmol graphene oxide ultrasonic disperse in 60 mL deionized waters, add the 0.4 mL ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate schematic diagram of Fig. 1 (its structure see), and be sufficiently stirred for, then sequentially add 0.76 g (6.25 mmol) Cys and 0.3 g (1.25 mmol) sodium molybdate (Na2MoO42H2O), and it is stirred continuously and makes Cys and sodium molybdate be completely dissolved, adjust volume to about 80 mL with deionized water；
2) obtained mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, this reactor is put in constant temperature oven, at 240 DEG C after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, collect solid product with centrifugation, and fully wash with deionized water, it is vacuum dried at 100 DEG C, by obtained hydro-thermal solid product in nitrogen/hydrogen mixed gas atmosphere at 500 DEG C heat treatment 2h, in mixed gas, the volume fraction of hydrogen is 10%, prepares multiple edge MoS2The composite nano materials of nanometer sheet/Graphene, multiple edge MoS in composite nano materials2Nanometer sheet is 1:2 with the ratio of the amount of Graphene material, obtains multiple edge MoS with XRD, SEM and TEM to prepared2The composite nano materials of nanometer sheet/Graphene characterizes, and characterization result display composite nano materials is accurate three-dimensional loose structure, MoS therein2Being the nanometer sheet of few number of plies multiple edge, its number of plies is at 3-6 layer, and the average number of plies is 4 layers (see Fig. 2 and Fig. 3)；
3) by the multiple edge MoS of above-mentioned preparation2Nanometer sheet/graphene composite nano material is as the active substance of electrochemistry storage magnesium, with acetylene black, the N-Methyl pyrrolidone solution of the Kynoar of carboxymethyl cellulose and mass fraction 5% is under agitation sufficiently mixed the uniform slurry of furnishing, this uniform slurry is coated onto equably on the foam copper of collector, it is vacuum dried at 120 DEG C, to multiple edge MoS after rolling2/ Graphene electrochemistry storage magnesium combination electrode, in combination electrode, each component and mass percent are: multiple edge MoS2Nanometer sheet/graphene composite nano material 80%, acetylene black 10%, carboxymethyl cellulose 5%, Kynoar 5%.
Electrochemistry storage magnesium performance test: with multiple edge MoS2/ Graphene electrochemistry storage magnesium combination electrode is working electrode, and with metal magnesium sheet as to electrode, electrolyte is the Mg [AlCl of 0.25 mol/L2(C4H9)(C2H5)]2Tetrahydrofuran solution be electrolyte, porous polypropylene film (Celguard-2300) is barrier film, is assembled into test battery in the suitcase of full argon.Storing magnesium performance by the electrochemistry of constant current charge-discharge test compound electrode, charge and discharge cycles is carried out on programme controlled auto charge and discharge instrument, charging and discharging currents density 50 mA/g, voltage range 0.3 ~ 3.0 V.Electrochemical results shows: multiple edge MoS2The initial reversible capacity of/Graphene electrochemistry storage magnesium combination electrode is 263 mAh/g, and after 50 circulations, reversible capacity is 252 mAh/g, it is shown that high specific capacity and excellent stable circulation performance；When high current charge-discharge (charging and discharging currents is 800 mA/g), its capacity is 185 mAh/g, it is shown that the high power charging-discharging characteristic (comparing with following comparative example) that it is obviously enhanced.
Comparative example
Without ionic liquid, it is prepared for MoS by above-mentioned similar approach2Nanometer sheet/Graphene electrochemistry storage magnesium combination electrode, concrete preparation process is as follows:
By 2.5 mmol graphene oxide ultrasonic disperse in 60 mL deionized waters, then it is sequentially added into 0.76g (6.25 mmol) Cys and 0.3 g (1.25 mmol) sodium molybdate (Na2MoO42H2O), and be stirred continuously and make Cys and sodium molybdate be completely dissolved, with deionized water adjustment volume to about 80 mL, obtained mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, this reactor is put in constant temperature oven, at 240 DEG C after hydro-thermal reaction 24 h, it is allowed to naturally cool to room temperature, solid product is collected with centrifugation, and fully wash with deionized water, it is vacuum dried at 100 DEG C, by obtained hydro-thermal solid product in nitrogen/hydrogen mixed gas atmosphere at 500 DEG C heat treatment 2h, in mixed gas, the volume fraction of hydrogen is 10%, prepare MoS2The nano composite material of nanometer sheet/Graphene, MoS in composite nano materials2It is 1:2 with the ratio of the amount of the material of Graphene.With XRD, SEM and TEM to preparing MoS2The nano composite material of nanometer sheet/Graphene characterizes, characterization result display MoS2For the nanometer sheet of layer structure, the average number of plies is 6 layers (see Fig. 4 and Fig. 5).
By above-mentioned steps 3) process prepare MoS2Nanometer sheet/Graphene electrochemistry storage magnesium combination electrode, and test its electrochemistry storage magnesium performance by above-mentioned identical method.Electrochemical results shows: MoS2Nanometer sheet/Graphene electrochemistry storage magnesium combination electrode electrochemistry storage initial the reversible capacity of magnesium be 135 mAh/g(charging and discharging currents be 50 mA/g), after 50 circulations, reversible capacity is 125 mAh/g；When high current charge-discharge (charging and discharging currents is 800 mA/g), its capacity is 85 mAh/g.
Claims (2)
1. a multiple edge MoS2/ Graphene electrochemistry storage magnesium combination electrode, it is characterised in that the electrochemistry storage magnesium of described combination electrode
Active substance is the multiple edge MoS of few number of plies2The composite nano materials of nanometer sheet/Graphene, multiple edge in composite nano materials
MoS2The ratio of the amount of the material of nanometer sheet and Graphene is 1:2, and the component of combination electrode and mass percentage content thereof be: polygon
Edge MoS2Nanometer sheet/graphene composite nano material 80%, acetylene black 10%, carboxymethyl cellulose 5%, Kynoar 5%,
The preparation method of described combination electrode is carried out as follows:
(1) by graphene oxide ultrasonic disperse in deionized water, appropriate ionic liquid 1-butyl-3-methyl imidazolium Tetrafluoroboric acid is added
Salt ([BMIM] BF4), and it is sufficiently stirred for, then sequentially adds Cys and sodium molybdate, and be stirred continuously and make L-half Guang
Propylhomoserin and sodium molybdate are completely dissolved, and the ratio of the amount of the material of Cys and sodium molybdate consumption is 5:1, sodium molybdate and graphite oxide
The ratio of the amount of the material of alkene is 1:2；
(2) mixed dispersion that step (1) obtains is transferred in hydrothermal reaction kettle, and add deionized water adjustment volume to water
The 80% of thermal response still nominal volume, the content of ionic liquid is 5mL/L, puts in constant temperature oven by this reactor, at 240 DEG C
After lower hydro-thermal reaction 24h, allow it naturally cool to room temperature, collect hydro-thermal solid product with centrifugation, and fill with deionized water
Dividing washing, be vacuum dried at 100 DEG C, obtained hydro-thermal solid product is warm at 500 DEG C in nitrogen/hydrogen mixed gas atmosphere
Processing 2h, in mixed gas, the volume fraction of hydrogen is 10%, prepares multiple edge MoS2The compound of nanometer sheet/Graphene is received
Rice material；
(3) by the multiple edge MoS of above-mentioned preparation2Nanometer sheet/graphene composite nano material stores magnesium active matter as the electrochemistry of electrode
Matter, with the N-Methyl pyrrolidone solution of the Kynoar of acetylene black, carboxymethyl cellulose and mass fraction 5% under agitation
It is sufficiently mixed the uniform slurry of furnishing, this slurry is coated onto equably on the foam copper of collector, be dried, prepare after rolling
Obtain multiple edge MoS2/ Graphene electrochemistry storage magnesium combination electrode.
Multiple edge MoS the most according to claim 12/ Graphene electrochemistry storage magnesium combination electrode, it is characterised in that described polygon
Edge MoS2The number of plies of nanometer sheet is 3～6 layers.
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| CN102701192A (en) * | 2012-06-08 | 2012-10-03 | 浙江大学 | Method for preparing monolayer MoS2 and graphene compounded nano material |
| CN102698774A (en) * | 2012-06-08 | 2012-10-03 | 浙江大学 | Hydrothermal preparation method for single-layer MoS2 and graphene composite nano material |
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