CN109686954A - A kind of C-O-Mo key bridge joint monolithic taper MoS2/ NG sodium ion negative electrode material and preparation method thereof - Google Patents
A kind of C-O-Mo key bridge joint monolithic taper MoS2/ NG sodium ion negative electrode material and preparation method thereof Download PDFInfo
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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- H—ELECTRICITY
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Abstract
The present invention discloses a kind of long circulating high magnification C-O-Mo key bridge joint monolithic taper MoS2/ NG sodium ion negative electrode material and preparation method thereof, promote the formation of C-O-Mo key using N-methyl pyrrolidones as " sacrifice agent ", so that bridge joint of the molybdenum disulfide of monolithic pyramidal structure self assembly by chemical bond, to be fixed on nitrogen-doped graphene flexibility base.This method has the characteristics that preparation process is simple, the period is short, low energy consumption, reproducible and yield is high.The MoS prepared using this method2The monolithic tapered structure of/NG relies on this principle of the stability of triangle, so that material has the stabilization function of self-supporting；The C-O-Mo key bridged from NMP molecule is fixed on NG, has more consolidated the growth of molybdenum disulfide on the surface of graphene on the basis of improving material overall conductivity.The composite material makes sodium ion electrode have high capacity conservation rate and excellent high rate performance, even if in 5A g‑1Current density under, 1000 times circulation after capacity still can reach 151mAh g‑1。
Description
Technical field
The present invention relates to sodium-ion battery technical fields more particularly to a kind of length to follow bad high magnification C-O-Mo key bridge joint monolithic
Taper MoS2/ NG sodium ion negative electrode material and preparation method thereof.
Background technique
As scarcity of resources, energy crisis and pollution pressure are increasingly sharpened, find a kind of efficient clean energy resource at
For the focus of various countries, and use and develop secondary rechargeable battery be it is most effective so far, most can solve the energy and environment danger
A kind of necessary mode of machine.Wherein, sodium-ion battery (SIBs) is a kind of electrochemical energy storage power supply, there are raw material resources to enrich,
It is cheap, specific energy is high, the advantages that having a safety feature.And sodium and lithium at same main group (IA) there is similar structure to make
It is almost the same in performance.Compared with lithium ion battery (LIBs), it is advantageous that resourceful be easy to get, it is low in cost；
SIBs has various excellent properties and metastable chemical property, and in business, replaces LIBs that will make into SIBs
This reduction about 30%, so that it is expected to replace LIBs in energy storage field.Graphite is used as the main anode material of business SIBs at present
Material.However, when graphite is used as SIB anode material, the big Na of ionic radius+The reaction of (0.106nm) and Na related electrode is delayed
Slow kinetics feature leads to the low rate ability and low capacity (about 25mAhg of SIBs-1)([1]J.B.Li,J.L.Li,D.Yan,
S.J.Hou,X.T.Xu,T.Lu,Y.F.Yao,W.J.Mai andL.K.Pan,J.Mater.Chem.A,2018,5,6595-
6605.[2]D.Y.Yu,P.V.Prikhodchenko,C.W.Mason,S.K.Batabyal,J.Gun,S.Sladkevich,
A.G.Medvedev and O.Lev,Nat.Commun.,2013,4,2922.).In addition, Na+Insertion-abjection process easily draw
Host lattice structural collapse is played, causes the cycle performance of material, electrochemical utilization rate poor, therefore, finds suitable embedding sode cell
Material has certain difficulty.
Sodium rice grade metallic compound MoS2, theoretical capacity with higher.MoS2With sandwich with S-Mo-S as graphite-phase
Layer structure, S atom and Mo atom are with Covalent bonding together in layer, and Mo-S faceted pebble is quite a lot of, large specific surface area, and layer edge has vacantly
Key.There are many lattice vacancies for this layer structure, can be used as the host lattice of intercalation.However, the MoS of 2D2Sodium rice piece inclines
Cause capacity in cyclic process significant in the accumulation again and aggregation that attract driving by interlayer Van der Waals force and high surface energy
Decaying.Meanwhile reaction intermediate (Na2S it) can dissolve in the electrolyte, this not only results in the loss of active material, can also be rotten
Lose electrode.In storage sodium negative electrode material, carbon based negative electrodes material is the most commonly used material of research.Carbon material is as conductive matrices
Solve MoS2Available strategy ([3] W.Ren, W.Zhou, H.Zhang and C.Cheng, ACS of these problems
Appl.Mater.Interfaces,2016,9,487-495.).Graphene is due to its big surface area, surface function abundant
Group, excellent mechanical stability and electric conductivity, as building MoS2The ideal composition of/graphene and receive more and more attention
([4]Y.Li,H.Wang,L.Xie,Y.Liang,G.Hong and H.Dai,J.Am.Chem.Soc.,2011,133,7296-
7299).In addition, the adjustable electronic structure of impurity doped graphene, increases chemical activity, enhance between carbon and active material
Connection ([5] T.Shan, S.Xin, Y.You, H.P.Cong, S.H.Yu and A.Manthiram,
Angew.Chem.Int.Ed.,2016,128,12975-12980).Secondly the advantages of this carbon material, is in original material
On the basis of form the pore structure of multistage distribution, increase the contact area of electrolyte and material, provided for electrolyte-electrode interface
Extensive percolating network shortens ion diffusion path ([6] Z.Chen, W.Ren, L.Gao, B.Liu, S.Pei and
H.M.Cheng,Nat.Mater.,2011,10,424-428.R.Mo,D.Rooney,K.Sun and H.Y.Yang,
Nat.Commun.,2017,8,13949.).Therefore, porous MoS is prepared2Structure is a kind of very promising improved method.
Summary of the invention
The purpose of the present invention is to provide a kind of long circulating high magnification C-O-Mo keys to bridge monolithic taper MoS2/ NG sodium ion
Negative electrode material and preparation method thereof.The preparation method is easily-controllable easy to operate, and yield is high, and the period is short, prepared electrode material tool
There are high capacity conservation rate and excellent high rate performance.
In order to achieve the above objectives, preparation method of the invention the following steps are included:
1) GO of 0.01~0.05g is distributed in 50mL deionized water and obtains solution A；
2) by the H of 2~3g2CNSNH2It is added in solution A and stirs evenly to obtain solution B；
3) by the MoO of 0.2~0.5g3It is added in solution B, stirring to MoO3It is completely dissolved, resulting dispersion C；
4) nmp solution of 2~8ml is slowly added into dispersion C and stirs to obtain gluey navy blue performed polymer D；
5) under inert gas protection, performed polymer D is placed in magnetic boat, is put into horizontal pipe furnace with 1~10 DEG C of min-1
Heating rate be heated to 500~800 DEG C of heat preservation to tubular type furnace temperatures from room temperature and reach 100 DEG C, close inert gas flow, then
It is cooled to room temperature, obtains product E；
6) after cleaning product E with deionized water and ethyl alcohol respectively, freeze-drying obtains C-O-Mo key bridge joint monolithic taper
MoS2/ NG sodium ion negative electrode material.
The step 2) stirring is magnetic agitation at room temperature.
Step 4) the stirring is stirred at 100 DEG C.
The inert gas of the step 5) uses argon gas.
Deionized water and the ethyl alcohol cleaning of the step 5) are respectively washed 3-5 times.
Press the bridge joint of C-O-Mo key made of method made above monolithic taper MoS2/ NG sodium ion negative electrode material is adulterated in N-
Graphene oxide substrate NG on monolithic MoS2It is self-assembled into pyramidal structure and the hole with 50-100nm, in 5Ag-1Big electricity
Under current density, material capacity after 1000 circulations is 151mAh g-1。
The present invention follows bad high magnification C-O-Mo key bridge joint monolithic taper MoS by the way that solid phase in-situ sintering method one-step synthesis is long2/
NG sodium ion negative electrode material.Monolithic MoS on N-doped graphene oxide substrate (NG)2It is self-assembled into pyramidal structure and tool
Having size range is the hole of 50-100nm, shows good mechanical stability.Introduce a small amount of n-methyl-2-pyrrolidone
(NMP) solution is to promote monolithic taper MoS2The formation of C-O-Mo key between the interface NG is improving material overall conductivity
On the basis of more consolidated the growth of molybdenum disulfide on the surface of graphene.This method is used as sodium ion main body for effectively constructing
The monolithic tapered, porous MoS of material2/ NG structure.Even if in 5A g-1High current density under, the material 1000 times circulation after
Also reach 151mAh g-1High capacity.
Detailed description of the invention
Fig. 1 is the SEM spectrum for the negative electrode material that the present invention prepares.
Fig. 2 is the XPS micrograph for the negative electrode material that the present invention prepares, and abscissa is bond energy in figure, ordinate is intensity.
Fig. 3 is the high rate performance map for the negative electrode material that the present invention prepares, and abscissa is circulating ring number, ordinate in figure
For capacity.
Fig. 4 is the cycle performance map for the negative electrode material that the present invention prepares, and abscissa is circulating ring number in figure, the left side is indulged
Coordinate is capacity, and right ordinate scale is coulombic efficiency.
Specific embodiment
The present invention is described in further detail in conjunction with specific embodiments, it is described be explanation of the invention rather than
It limits.
Embodiment 1:
1) GO of 0.03g (graphene oxide) is distributed in 50mL deionized water and obtains solution A；
2) by the H of 2.8g2CNSNH2(thiocarbamide) be added to room temperature magnetic agitation in solution A it is uniform solution B；
3) by the MoO of 0.28g3It is added in solution B, stirring to MoO3It is completely dissolved, resulting dispersion C；
4) NMP of 3.3ml (n-methyl-2-pyrrolidone) solution is slowly added into dispersion C at 100 DEG C and is stirred
Gluey navy blue performed polymer D；
5) under inert gas argon gas shielded, performed polymer D is placed in magnetic boat, is put into horizontal pipe furnace with 5 DEG C of min-1
Heating rate be heated to 600 DEG C of heat preservation to tubular type furnace temperatures from room temperature and reach 100 DEG C, close argon gas stream, be subsequently cooled to room
Temperature obtains product E；
6) after product E being cleaned 5 times with deionized water and ethyl alcohol respectively, freeze-drying obtains C-O-Mo key bridge joint monolithic cone
Shape MoS2/ NG sodium ion negative electrode material.
Embodiment 2:
1) GO of 0.05g (graphene oxide) is distributed in 50mL deionized water and obtains solution A；
2) by the H of 2.7g2CNSNH2(thiocarbamide) be added to room temperature magnetic agitation in solution A it is uniform solution B；
3) by the MoO of 0.3g3It is added in solution B, stirring to MoO3It is completely dissolved, resulting dispersion C；
4) NMP of 3ml (n-methyl-2-pyrrolidone) solution is slowly added into dispersion C and stirs to obtain glue at 100 DEG C
Shape navy blue performed polymer D；
5) under inert gas argon gas shielded, performed polymer D is placed in magnetic boat, is put into horizontal pipe furnace with 5 DEG C of min-1
Heating rate be heated to 650 DEG C of heat preservation to tubular type furnace temperatures from room temperature and reach 100 DEG C, close argon gas stream, be subsequently cooled to room
Temperature obtains product E；
6) after product E being cleaned 5 times with deionized water and ethyl alcohol respectively, freeze-drying obtains C-O-Mo key bridge joint monolithic cone
Shape MoS2/ NG sodium ion negative electrode material.
Embodiment 3:
1) GO of 0.03g (graphene oxide) is distributed in 50mL deionized water and obtains solution A；
2) by the H of 2.6g2CNSNH2(thiocarbamide) be added to room temperature magnetic agitation in solution A it is uniform solution B；
3) by the MoO of 0.33g3It is added in solution B, stirring to MoO3It is completely dissolved, resulting dispersion C；
4) NMP of 3ml (n-methyl-2-pyrrolidone) solution is slowly added into dispersion C and stirs to obtain glue at 100 DEG C
Shape navy blue performed polymer D；
5) under inert gas argon gas shielded, performed polymer D is placed in magnetic boat, is put into horizontal pipe furnace with 10 DEG C of min-1
Heating rate be heated to 700 DEG C of heat preservation to tubular type furnace temperatures from room temperature and reach 100 DEG C, close argon gas stream, be subsequently cooled to room
Temperature obtains product E；
6) after product E being cleaned 5 times with deionized water and ethyl alcohol respectively, freeze-drying obtains C-O-Mo key bridge joint monolithic cone
Shape MoS2/ NG sodium ion negative electrode material.
Embodiment 4:
1) GO of 0.04g (graphene oxide) is distributed in 50mL deionized water and obtains solution A；
2) by the H of 2.5g2CNSNH2(thiocarbamide) be added to room temperature magnetic agitation in solution A it is uniform solution B；
3) by the MoO of 0.35g3It is added in solution B, stirring to MoO3It is completely dissolved, resulting dispersion C；
4) NMP of 5ml (n-methyl-2-pyrrolidone) solution is slowly added into dispersion C and stirs to obtain glue at 100 DEG C
Shape navy blue performed polymer D；
5) under inert gas argon gas shielded, performed polymer D is placed in magnetic boat, is put into horizontal pipe furnace with 10 DEG C of min-1
Heating rate be heated to 750 DEG C of heat preservation to tubular type furnace temperatures from room temperature and reach 100 DEG C, close argon gas stream, be subsequently cooled to room
Temperature obtains product E；
6) after product E being cleaned 5 times with deionized water and ethyl alcohol respectively, freeze-drying obtains C-O-Mo key bridge joint monolithic cone
Shape MoS2/ NG sodium ion negative electrode material.
Embodiment 5:
1) GO of 0.01g (graphene oxide) is distributed in 50mL deionized water and obtains solution A；
2) by the H of 2g2CNSNH2(thiocarbamide) be added to room temperature magnetic agitation in solution A it is uniform solution B；
3) by the MoO of 0.2g3It is added in solution B, stirring to MoO3It is completely dissolved, resulting dispersion C；
4) NMP of 5ml (n-methyl-2-pyrrolidone) solution is slowly added into dispersion C and stirs to obtain glue at 100 DEG C
Shape navy blue performed polymer D；
5) under inert gas argon gas shielded, performed polymer D is placed in magnetic boat, is put into horizontal pipe furnace with 1 DEG C of min-1
Heating rate be heated to 500 DEG C of heat preservation to tubular type furnace temperatures from room temperature and reach 100 DEG C, close argon gas stream, be subsequently cooled to room
Temperature obtains product E；
6) after product E being cleaned 3 times with deionized water and ethyl alcohol respectively, freeze-drying obtains C-O-Mo key bridge joint monolithic cone
Shape MoS2/ NG sodium ion negative electrode material.
Embodiment 6:
1) GO of 0.05g (graphene oxide) is distributed in 50mL deionized water and obtains solution A；
2) by the H of 3g2CNSNH2(thiocarbamide) be added to room temperature magnetic agitation in solution A it is uniform solution B；
3) by the MoO of 0.5g3It is added in solution B, stirring to MoO3It is completely dissolved, resulting dispersion C；
4) NMP of 8ml (n-methyl-2-pyrrolidone) solution is slowly added into dispersion C and stirs to obtain glue at 100 DEG C
Shape navy blue performed polymer D；
5) under inert gas argon gas shielded, performed polymer D is placed in magnetic boat, is put into horizontal pipe furnace with 8 DEG C of min-1
Heating rate be heated to 800 DEG C of heat preservation to tubular type furnace temperatures from room temperature and reach 100 DEG C, close argon gas stream, be subsequently cooled to room
Temperature obtains product E；
6) after product E being cleaned 4 times with deionized water and ethyl alcohol respectively, freeze-drying obtains C-O-Mo key bridge joint monolithic cone
Shape MoS2/ NG sodium ion negative electrode material.
As can be seen from Figure 1 the form for the negative electrode material that the present invention prepares shows pyramidal structure, by NG base
The several ultra-thin MoS grown on bottom2Sodium rice piece is constituted, the hole for being 50-100nm with size range.
Referring to fig. 2, monolithic taper MoS is had studied by x-ray photoelectron spectroscopy2The surface composition and chemistry of/NG structure
State.It can be seen from the figure that peak value be respectively 533.1 and 531.2eV prove there are C-OH and C=O, after fitting
There is an absorption peak in 532.1eV, it means that there are C-O-Mo, due in the C=O key and MoS of NMP Molecular Ring2Mo
Recombination between formed.
Referring to Fig. 3, the negative electrode material that the present invention prepares under various current densities is applied to sodium-ion battery cathode material
The cycle performance figure of material.It can be seen from the figure that when electric current is restored to 0.05A g-1When, capacity can reach 376mAh g-1.It is excellent
Different sodium ion storage performance is attributable to the MoS wherein assembled2Sodium rice piece has monolithic countersunk arrangement and is fixed on the soft of NG
Structure on property supporter.Wherein C-O-Mo key is conducive to its structural stability.
Referring to fig. 4, it when the negative electrode material that the present invention prepares is applied to anode material of lithium-ion battery, shows excellent
Electrochemical stability.Even if in 5A g-1Current density under, 1000 times circulation after capacity still can reach 151mAh g-1, performance
Higher specific capacity and preferable cyclical stability out.
Claims (6)
1. a kind of C-O-Mo key bridges monolithic taper MoS2The preparation method of/NG sodium ion negative electrode material, it is characterised in that:
1) GO of 0.01~0.05g is distributed in 50mL deionized water and obtains solution A；
2) by the H of 2~3g2CNSNH2It is added in solution A and stirs evenly to obtain solution B；
3) by the MoO of 0.2~0.5g3It is added in solution B, stirring to MoO3It is completely dissolved, resulting dispersion C；
4) nmp solution of 2~8ml is slowly added into dispersion C and stirs to obtain gluey navy blue performed polymer D；
5) under inert gas protection, performed polymer D is placed in magnetic boat, is put into horizontal pipe furnace with 1~10 DEG C of min-1Liter
Warm rate is heated to 500~800 DEG C of heat preservation to tubular type furnace temperatures from room temperature and reaches 100 DEG C, closes inert gas flow, then cools down
To room temperature, product E is obtained；
6) after cleaning product E with deionized water and ethyl alcohol respectively, freeze-drying obtains C-O-Mo key bridge joint monolithic taper MoS2/
NG sodium ion negative electrode material.
2. C-O-Mo key according to claim 1 bridges monolithic taper MoS2/ NG sodium ion negative electrode material and its preparation side
Method, it is characterised in that: the step 2) stirring is magnetic agitation at room temperature.
3. C-O-Mo key according to claim 1 bridges monolithic taper MoS2/ NG sodium ion negative electrode material and its preparation side
Method, it is characterised in that: the step 4) stirring is stirred at 100 DEG C.
4. C-O-Mo key according to claim 1 bridges monolithic taper MoS2/ NG sodium ion negative electrode material and its preparation side
Method, it is characterised in that: the inert gas of the step 5) uses argon gas.
5. C-O-Mo key according to claim 1 bridges monolithic taper MoS2/ NG sodium ion negative electrode material and its preparation side
Method, it is characterised in that: deionized water and the ethyl alcohol cleaning of the step 5) are respectively washed 3-5 times.
6. a kind of C-O-Mo key as made of any one of claim 1-5 preparation method bridges monolithic taper MoS2/ NG sodium from
Sub- negative electrode material, it is characterised in that: the monolithic MoS on N-doped graphene oxide substrate NG2It is self-assembled into pyramidal structure
And the hole with 50-100nm, in 5Ag-1High current density under, the material 1000 times circulation after capacity be 151mAh g-1。
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| CN113745508A (en) * | 2021-09-03 | 2021-12-03 | 陕西科技大学 | Tremella-like MoS2Functionalized activated carbon sodium ion battery cathode material and preparation method thereof |
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