CN106033810A - MoS2 / graphene composite material and preparation method thereof - Google Patents
MoS2 / graphene composite material and preparation method thereof Download PDFInfo
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- CN106033810A CN106033810A CN201510111969.0A CN201510111969A CN106033810A CN 106033810 A CN106033810 A CN 106033810A CN 201510111969 A CN201510111969 A CN 201510111969A CN 106033810 A CN106033810 A CN 106033810A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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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
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Abstract
The invention relates to a MoS2 / graphene composite material and a preparation method thereof. The preparation method comprises the following steps: 1) weighing MoS2 and worm graphite as raw material powders; 2) milling the raw material powders to obtain the MoS2 / graphene composite material. The invention discloses the preparation method of the MoS2 / graphene composite material. The MoS2 / graphene composite material prepared by ball milling method; and the method is simple, low in cost and easy for macro preparation. The obtained composite material has excellent performance in application to cathode of lithium ion battery.
Description
Technical field
The present invention relates to a kind of field of compound material, more particularly to a kind of MoS2The preparation method of/graphene composite material,
It is mainly used in the fields such as lithium ion battery negative material.
Background technology
Along with the requirement of battery is carried by being widely used of lithium rechargeable battery, daily life and work the most day by day
Height, such as high security and high energy storage density.Overcome the safety problem of lithium ion battery, replace inflammable with the solid electrolyte not fired
Conventional liq electrolyte be the most effective approach.
At present, in solid electrolyte, sulfenyl solid electrolyte has higher lithium ion conductivity, is that ratio has wide application prospects
Liquid electrolyte substitution material.The negative material being all sulfide has good matching with sulfenyl solid electrolyte.For
Improving the high energy storage density of lithium ion battery, the capacity of the most conventional carbon negative pole material is only 370mAh/g, is far smaller than existing
The capacity of some the sulfide negative materials having been found that.The MoS of its sandwich2The capacity of (molybdenum bisuphide) can reach
More than 1000mAh/g.Additionally, the characteristic of high-lithium ion diffusion and satisfactory electrical conductivity makes MoS2There is high magnification capacity, with
And high cyclical stability.
But in battery practical work process, due to MoS2Volumetric expansion can cause certain capacity attenuation, thus shadow
Ring the overall performance of battery.To this end, have people to MoS2Carry out being combined with material with carbon element carrying out performance improvement, wherein with material with carbon element stone
After ink alkene forms composite negative pole material, its cyclical stability is significantly enhanced.But whether be in document before is reported
[Jin Wang,Advanced Materials,2014,26,7162-7169；Viet Hung Pham,Journal of Power Sources
2013,244,280-286] or in patent application [201210437583.5,201310006171.0,201410141470.X],
MoS2It is substantially employing liquid phase method with the complex method of Graphene, thus causes process complexity, cost high, it is important that
It is not easy to magnanimity prepare.In sum, the MoS that this area lacks a kind of simple, low cost, can be mass-produced2/ Graphene
The preparation method of composite.
Summary of the invention
It is contemplated that overcome existing MoS2/ graphene composite material defect in terms of preparation method, the invention provides one
Plant MoS2The preparation method of/graphene composite material.
The invention provides a kind of MoS2The preparation method of/graphene composite material, including:
1) MoS is weighed2, anthelmintic graphite is as material powder；
2) material powder is carried out ball-milling treatment, obtain described MoS2/ graphene composite material.
It is preferred that in material powder, MoS2, the mass ratio of anthelmintic graphite be x:1,2.5≤x≤20.
It is preferred that the technological parameter of ball-milling treatment includes:
The mass ratio of abrading-ball and material powder is y:(x+1), 4≤y≤40, drum's speed of rotation is 120 480r/ minute, ball milling
Time is 2～24 hours.
It is preferred that described MoS2In/graphene composite material, graphene coated is at MoS2Surface or MoS2Nanometer thin
Sheet is dispersed in graphene platelet surface.
The present invention also provides for MoS prepared by a kind of said method2/ graphene composite material, wherein in the multiplying power of 1Ah/g
Under, use described MoS2Battery capacity prepared by/graphene composite material can reach 550-600mAh/g.
Beneficial effects of the present invention:
The invention discloses a kind of MoS2The preparation method of/graphene composite material, utilizes ball-milling method to prepare MoS2/ Graphene composite wood
Material, not only method is simple, with low cost, be prone to magnanimity prepares, and when obtaining composite application with lithium ion battery negative
Excellent performance.
Accompanying drawing explanation
Fig. 1 shows the MoS of preparation in embodiment 12The stereoscan photograph of/graphene composite material；
Fig. 2 shows the MoS of preparation in embodiment 12The transmission electron microscope photo of/graphene composite material；
Fig. 3 shows the MoS of preparation in embodiment 12When/graphene composite material is used as negative material, the charge and discharge under different multiplying
Electricity loop test result.
Detailed description of the invention
The present invention is further illustrated, it should be appreciated that accompanying drawing and following embodiment are only below in conjunction with accompanying drawing and following embodiment
For the present invention is described, and the unrestricted present invention.
In order to realize simple, low cost, can magnanimity prepare, the present invention proposes a kind of MoS2The preparation of/graphene composite material
Method, only with MoS2Powder body and anthelmintic graphite are raw material, are then passed through ball milling and obtain MoS2/ Graphene is calculated as composite wood
Material.
The present invention provides a kind of MoS2The preparation method of/graphene composite material, preparation method of the present invention operation is simple, cost
Cheap, be prone to magnanimity and prepare MoS2/ graphene composite material.
Described stone MoS2/ graphene composite material is by MoS2Powder body and anthelmintic graphite obtain after mixing and ball milling；
Described processing step is:
1., MoS is weighed according to the ratio being x:1 in mass ratio2With anthelmintic graphite, it is placed in ball grinder；
2., by y:(x+1) ball material mass ratio relation put into ball milling ball；
3., ball grinder is packaged, ball milling on ball mill；
4., ball milling open ball grinder after terminating, obtain MoS after separating with ball milling ball2/ graphene composite material.
Described mass ratio x:1, wherein, 2.5≤x≤20.
Described ball material mass ratio y:(x+1), wherein, 4≤y≤40.
Described Ball-milling Time is 2～24h.
The MoS obtained2In/graphene composite material, graphene uniform is closely coated on MoS2Surface or MoS2Nanometer
Thin slice is evenly dispersed in graphene platelet surface.MoS2When/graphene composite material is used as lithium ion battery negative material, 1
Under the charge-discharge magnification of Ah/g, battery capacity reaches 600mAh/g.
Beneficial effect
The invention discloses a kind of MoS2The preparation method of/graphene composite material, utilizes ball-milling method to prepare MoS2/ Graphene composite wood
Material, not only method is simple, with low cost, be prone to magnanimity prepares, and when obtaining composite application with lithium ion battery negative
Excellent performance.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following example are served only for this
Bright it is further described, it is impossible to being interpreted as limiting the scope of the invention, those skilled in the art is according to the present invention's
Some nonessential improvement and adjustment that foregoing is made belong to protection scope of the present invention.The technique ginseng that following example is concrete
Number etc. is the most only an example in OK range, in the range of i.e. those skilled in the art can be done suitably by explanation herein
Select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
Weigh 4g MoS respectively2Powder body and 0.4g anthelmintic graphite composite powder, be positioned in ball grinder；Weigh the ball milling ball of 20g, put
In ball grinder；Packaged ball grinder, carries out ball milling on ball mill；Drum's speed of rotation is 240r/ minute, ball milling 20h
After, open ball grinder, after separating ball milling ball, obtain MoS2/ graphene composite material.
Fig. 1 is the scanning electron microscope (SEM) photograph of the composite obtained, it can be seen that anthelmintic graphite is wholly absent；
Fig. 2 is the transmission electron microscope picture (a and b yardstick mark post is respectively 0.5um and 10nm) of the composite obtained, it can be seen that stone
Ink alkene uniform close is coated on MoS2Surface or MoS2Nano flake is evenly dispersed in graphene platelet surface.
By gained MoS2/ graphene composite negative pole and conductive agent acetylene black, binding agent Kynoar are by quality 8:1:
It is coated in copper foil after 1 mix homogeneously and makes negative plate.With lithium sheet as to electrode, Celgard 2502 film as barrier film, carbonic acid
Vinyl acetate (EC)+dimethyl carbonate (DMC)+hexafluoro phosphorus lithium (LiPF6) it is electrolyte, it is assembled into CR2016 button cell.
Under room temperature condition (25 ± 2 DEG C), battery is carried out constant current discharge test in 0.05 3.0V voltage range.Figure
3 is battery charge and discharge cycles test result under different multiplying, it can be seen that under the multiplying power of 1Ah/g, battery capacity reaches
600mAh/g.And MoS2Phosphorus content in/graphene composite negative pole is only 9.1%, much smaller than document 20 40wt%,
So the clean specific capacity of resultant battery adds.
Embodiment 2
Weigh 2g MoS respectively2Powder body and 0.4g anthelmintic graphite composite powder, be positioned in ball grinder；Weigh the ball milling ball of 20g, put
In ball grinder；Packaged ball grinder, carries out ball milling on ball mill；Drum's speed of rotation is 360r/ minute, ball milling 12h
After, open ball grinder, after separating ball milling ball, obtain MoS2/ graphene composite material；
Being assembled into battery testing to show, under the multiplying power of 1Ah/g, battery capacity reaches 580mAh/g.
Embodiment 3
Weigh 1g MoS respectively2Powder body and 0.4g anthelmintic graphite composite powder, be positioned in ball grinder；Weigh the ball milling ball of 20g, put
In ball grinder；Packaged ball grinder, carries out ball milling on ball mill；Drum's speed of rotation is 120r/ minute, ball milling 24h
After, open ball grinder, after separating ball milling ball, obtain MoS2/ graphene composite material；
Being assembled into battery testing to show, under the multiplying power of 1Ah/g, battery capacity reaches 580mAh/g.
Embodiment 4
Weigh 8g MoS respectively2Powder body and 0.4g anthelmintic graphite composite powder, be positioned in ball grinder；Weigh the ball milling ball of 60g, put
In ball grinder；Packaged ball grinder, carries out ball milling on ball mill；Drum's speed of rotation is 450r/ minute, ball milling 8h
After, open ball grinder, after separating ball milling ball, obtain MoS2/ graphene composite material；
Being assembled into battery testing to show, under the multiplying power of 1Ah/g, battery capacity reaches 550mAh/g.
Embodiment 5
Weigh 4g MoS respectively2Powder body and 0.4g anthelmintic graphite composite powder, be positioned in ball grinder；Weigh the ball milling ball of 120g, put
In ball grinder；Packaged ball grinder, carries out ball milling on ball mill；Drum's speed of rotation is 480r/ minute, ball milling 2h
After, open ball grinder, after separating ball milling ball, obtain MoS2/ graphene composite material；
Being assembled into battery testing to show, under the multiplying power of 1Ah/g, battery capacity reaches 590mAh/g.
Claims (5)
1. a MoS2The preparation method of/graphene composite material, it is characterised in that including:
1) MoS is weighed2, anthelmintic graphite is as material powder；
2) material powder is carried out ball-milling treatment, obtain described MoS2/ graphene composite material.
Preparation method the most according to claim 1, it is characterised in that in material powder, MoS2, the mass ratio of anthelmintic graphite be x:1,2.5≤x ≤20。
Preparation method the most according to claim 2, it is characterised in that the technological parameter of ball-milling treatment includes:
Abrading-ball with the mass ratio of material powder isy : (x, 4+1)≤
y≤ 40, drum's speed of rotation is 120 480r/ minute, and Ball-milling Time is 2～24 hours.
4. according to described preparation method arbitrary in claim 1-3, it is characterised in that described MoS2In/graphene composite material, graphene coated is at MoS2Surface or MoS2Nano flake is dispersed in graphene platelet surface.
5. the MoS prepared according to described preparation method arbitrary in claim 1-42/ graphene composite material, it is characterised in that under the multiplying power of 1 Ah/g, uses described MoS2Battery capacity prepared by/graphene composite material can reach 550-600 mAh/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510111969.0A CN106033810A (en) | 2015-03-13 | 2015-03-13 | MoS2 / graphene composite material and preparation method thereof |
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| CN201510111969.0A CN106033810A (en) | 2015-03-13 | 2015-03-13 | MoS2 / graphene composite material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107834051A (en) * | 2017-12-13 | 2018-03-23 | 常熟理工学院 | A kind of preparation method of lithium ion battery and electrode material for super capacitor |
| CN113675391A (en) * | 2021-08-05 | 2021-11-19 | 常熟理工学院 | Heterogeneous layered composite material for lithium ion battery cathode and preparation method thereof |
| US11208334B2 (en) | 2017-08-01 | 2021-12-28 | Iowa State University Research Foundation, Inc. | Preparation of metal chalcogenides |
| US11919781B2 (en) | 2017-08-01 | 2024-03-05 | Iowa State University Research Foundation, Inc. | Preparation of metal chalcogenides |
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| CN103022453A (en) * | 2013-01-10 | 2013-04-03 | 上海中聚佳华电池科技有限公司 | Lithium ion battery negative electrode material Si@SiOx/graphene composite and preparation method thereof |
| US20140121425A1 (en) * | 2012-07-27 | 2014-05-01 | Lawrence Livermore National Security, Llc | High surface area graphene-supported metal chalcogenide assembly |
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Patent Citations (3)
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| US20140121425A1 (en) * | 2012-07-27 | 2014-05-01 | Lawrence Livermore National Security, Llc | High surface area graphene-supported metal chalcogenide assembly |
| CN103022453A (en) * | 2013-01-10 | 2013-04-03 | 上海中聚佳华电池科技有限公司 | Lithium ion battery negative electrode material Si@SiOx/graphene composite and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11208334B2 (en) | 2017-08-01 | 2021-12-28 | Iowa State University Research Foundation, Inc. | Preparation of metal chalcogenides |
| US11919781B2 (en) | 2017-08-01 | 2024-03-05 | Iowa State University Research Foundation, Inc. | Preparation of metal chalcogenides |
| CN107834051A (en) * | 2017-12-13 | 2018-03-23 | 常熟理工学院 | A kind of preparation method of lithium ion battery and electrode material for super capacitor |
| CN107834051B (en) * | 2017-12-13 | 2020-05-15 | 常熟理工学院 | Preparation method of electrode material of lithium ion battery and super capacitor |
| CN113675391A (en) * | 2021-08-05 | 2021-11-19 | 常熟理工学院 | Heterogeneous layered composite material for lithium ion battery cathode and preparation method thereof |
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