CN102522542A - Elemental sulfur composite material containing graphene and preparation method thereof - Google Patents
Elemental sulfur composite material containing graphene and preparation method thereof Download PDFInfo
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Abstract
The invention provides an elemental sulfur composite material containing graphene and a preparation method of the composite material. The composite material is a binary material AxBy, wherein A is grapheme, and B is elemental sulfur, x is more than or equal to 1 percent and less than or equal to 90 percent while y is more than or equal to 10 percent and less than or equal to 99, and x plus y equals to 100 percent, and B is dispersed on the surface of A in a nanometer state. The preparation method comprises the steps of carrying out hydro-thermal treatment on the elemental sulfur and the graphene oxide between 50 and 500 degrees; and reducing the graphene oxide into the graphene by the elemental sulfur, and obtaining the elemental sulfur composite material containing grapheme of which nano-sulfur is uniformly dispersed on the surface of the grapheme at the same time. Lithium sulfur batteries or sodium sulfur batteries are prepared by using the composite material as an anode and a metal lithium or metal sodium as a cathode; moreover, the lithium sulfur batteries can be charged or discharged under the room temperature, and the reversibility specific capacity of the sulfur-based composite material containing grapheme is up to 1480mAh/g.
Description
Technical field
The present invention relates to a kind of positive electrode material for secondary battery and preparation method thereof, particularly a kind of secondary cell is with elemental sulfur composite positive pole and preparation method thereof.
Background technology
Along with the deterioration of the short serious day by day and amblent air temperature of global energy, people are more and more urgent to the demand of clean energy resource, and battery is being brought into play irreplaceable effect as the storage and the conversion equipment of energy in the process of clean energy resource utilization.Lithium ion battery is compared with other types secondary cell commonly used, because of it has very high specific energy with volumetric specific energy has very big advantage, has attracted concern widely.The secondary cell of low cost, high-energy-density, high security, long circulation life, environmental protection is a lithium battery hot of research and development of future generation.
The LiFePO4 of lithium transition-metal oxide that present commercial positive electrode mainly is stratiform or spinel structure (like cobalt acid lithium, LiMn2O4) and olivine structural etc.But, can not satisfy the requirement of high-energy density secondary battery of future generation because of reasons such as these positive electrode self structure and composition cause the shortcoming that capacity is lower, price is higher and fail safe is relatively poor.Elemental sulfur generates lithium sulfide (Li as positive electrode and lithium reaction
2S) theoretical capacity can be more than 6 times of conventional transition metal oxide or phosphoric acid salt positive electrode, and elemental sulfur be cheap, safety non-toxic up to 1672mAh/g, is the novel anode active material that has development potentiality.
Since the many decades; The inorganic sulphide of elemental sulfur and sulfur-bearing, organic disulfide, gather organic disulfide, organic polysulfide, gather the thioated thing and carbon-sulphur polymer etc. is extensively paid close attention to as the positive electrode of high power capacity, but still there are a lot of problems in these materials.At first, the conductivity of elemental sulfur and sulfide itself is very poor, must add a large amount of conductive agents to increase its conductivity.Secondly, concerning elemental sulfur as the positive pole of active material, though the Li of the elementary sulfur that exists on the positive pole when charging fully existence when discharging fully
2S is insoluble in the polarity organic electrolyte, but many lithium sulfides that positive pole contains when partial charging and discharge condition are soluble in the polarity organic electrolyte, and is same; The micromolecule sulfide that produces when gathering the organic sulfur compound discharge also is soluble in organic electrolyte, and in the negative pole deposition, influences the cycle performance (Kolosnitsyn of battery; V.S., Karaseva, E.V.Russian Journal of Electrochemistry 2008; 44 (5), pp.506-509).Therefore, how improving the conductivity of material, and solve the problems of dissolution that discharges and recharges intermediate product, improve cycle performance of battery, is the research emphasis of sulfenyl positive electrode.
Graphene is a kind of electronics and heat conductor with high-specific surface area, high chemical stability and high mechanical properties, with Graphene and elemental sulfur compound be the effective means that overcomes the above-mentioned shortcoming of elemental sulfur.Be dispersed in the surface of Graphene through simple substance sulphur granule, the high-specific surface area of Graphene can play the effect of absorption sulphur, and high electron conduction then can overcome the problem of elemental sulfur insulation.There is paper to report the synthetic method of Graphene-sulphur composite material (Hailiang Wang, Yuan Yang, Yi Cui, and Hongjie Dai.Nano Letters 2011,11,2644-2647 recently; Jiazhao Wang, Lin Lu, Xun Xu; Huakun Liu.Journal of Power Sources 2011,196,7030-7034); Comparing cycle performance with elemental sulfur has had certain improvement, but also exists complicated process of preparation, and compound many shortcomings such as inhomogeneous have much room for improvement and improve.
Summary of the invention
The present invention is directed to the above-mentioned deficiency that exists in the prior art, elemental sulfur composite material of a kind of graphitiferous alkene and preparation method thereof is provided.
The present invention realizes through following technical scheme.
A kind of elemental sulfur composite material of graphitiferous alkene, said composite material are the binary composite A
xB
y, wherein, A is a Graphene, and B is an elemental sulfur, and B is dispersed in the A surface with the nanometer state, and wherein, x, y are respectively the content of Graphene and elemental sulfur, said 1%≤x≤90%, said 10%≤y≤99%, and x+y=100%.
The preparation method of the elemental sulfur composite material of a kind of preparation as graphitiferous alkene according to claim 1 comprises the steps:
Step 1 adds graphene oxide in the deionized water, makes the dispersion liquid of graphene oxide;
Step 2 adds elemental sulfur, obtains the mixture paste of graphene oxide and elemental sulfur;
Step 3, mixture paste carried out heat treated after, washing filtering obtains the elemental sulfur composite material of graphitiferous alkene.
Said graphene oxide thickness is 0.35～3.5nm, wherein comprises 1～10 graphite flake layer, and said graphite flake layer length and width is respectively 10nm～10 μ m.
In step 1, said graphene oxide is 1 mass parts.
In step 1, said deionized water is the 1-500 mass parts.
In step 2, said elemental sulfur is the 0.1-30 mass parts.
In step 3, said heat treated is handled in polytetrafluoroethylene that seals or stainless cylinder of steel, carrying out hydro thermal method.
In step 3, said heat treated corresponding temperature is 50～500 ℃.
In step 3, the corresponding time of said heat treated is 1～72 hour.
The elemental sulfur composite material of graphitiferous alkene provided by the invention has following advantage:
Evenly compound at structure aspects binary composite material; Elemental sulfur is dispersed in the surface of the Graphene that obtains of reduction with the nanometer state; This structure helps when being used for cell positive material, giving full play to the high conductivity of Graphene and to the stabilization of material structure, improves the power characteristic of battery; The high thermal conductivity of Graphene helps the heat radiation of composite material, and high-specific surface area helps many lithium sulfides of producing in the sorption cycle process, and these character play an important role to the cyclical stability that improves battery.The nanometer sulphur size that is dispersed in the Graphene surface is less, helps making full use of of sulphur, improves the utilance of elemental sulfur in composite material, promptly improves the energy density of composite material.
The preparation method of the elemental sulfur composite material of graphitiferous alkene provided by the invention has following advantage:
Utilize the hydro thermal method elemental sulfur that graphene oxide is carried out in-situ reducing, simultaneously elemental sulfur is evenly distributed on the surface of Graphene with the nanometer state, and it is simple to have synthetic method, the material pattern the is adjustable controlled remarkable advantage that waits.
Adopt positive pole and lithium metal or the sodium metal negative pole composition lithium-sulfur rechargeable battery or the sodium-sulfur secondary battery of the present invention's preparation.At room temperature discharge and recharge, lithium-sulfur rechargeable battery can reach 1480mAh/g with the reversible capacity of elemental sulfur composite positive pole, and this material has excellent cycle performance.
Description of drawings
Fig. 1 is the SEM photo of the elemental sulfur composite material of the graphitiferous alkene that obtains by embodiment 3.
Fig. 2 is the charging and discharging curve of the elemental sulfur composite material of the graphitiferous alkene that obtains by embodiment 3.
Fig. 3 is the cycle performance curve of the elemental sulfur composite material of the graphitiferous alkene that obtains by embodiment 3.
Embodiment
Elaborate in the face of embodiments of the invention down: present embodiment provided detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Embodiment 1
Present embodiment provides a kind of elemental sulfur composite material of graphitiferous alkene, and this composite material is the binary composite A
xB
y, wherein, A is a Graphene, and B is an elemental sulfur, and B is dispersed in the A surface with the nanometer state, wherein, 1%≤x≤90%, 10%≤y≤99%, and x+y=100%.
The preparation method embodiment of the elemental sulfur composite material of the graphitiferous alkene that following examples provide for embodiment 1.
Embodiment 2
Present embodiment provides the preparation method of the elemental sulfur composite material of the graphitiferous alkene that a kind of embodiment of preparation 1 provides, and comprises the steps:
Step 1 adds graphene oxide in the deionized water, makes the dispersion liquid of graphene oxide; Be specially, the graphene oxide of 1 mass parts is added in the 1 mass parts deionized water, make the dispersion liquid of graphene oxide;
Step 2 adds elemental sulfur, obtains the mixture paste of graphene oxide and elemental sulfur; Be specially, add the elemental sulfur of 1 mass parts, obtain the mixture paste of graphene oxide and elemental sulfur;
Step 3, mixture paste carried out heat treated after, washing filtering obtains the elemental sulfur composite material of graphitiferous alkene; Be specially, 200 ℃ of heat treatments are after 24 hours in the teflon seal jar with mixture paste, and washing filtering obtains the elemental sulfur composite material of graphitiferous alkene, and wherein the mass content of Graphene is 50%, and the elemental sulfur mass content is 50%.
Embodiment 3
Embodiment 3 is the variant of embodiment 2, is specially:
Step 1 adds the graphene oxide of 1 mass parts in the 10 mass parts deionized waters, makes the dispersion liquid of graphene oxide;
Step 2 adds the elemental sulfur of 3 mass parts, obtains the mixture paste of graphene oxide and elemental sulfur;
Step 3,155 ℃ of heat treatments are after 48 hours in the teflon seal jar with mixture paste, and washing filtering obtains the elemental sulfur composite material of graphitiferous alkene, and wherein the mass content of Graphene is 20%, and the elemental sulfur mass content is 80%.
Embodiment 4
Embodiment 4 is the variant of embodiment 3, is specially:
Step 1 adds the graphene oxide of 1 mass parts in the 500 mass parts deionized waters, makes the dispersion liquid of graphene oxide;
Step 2 adds the elemental sulfur of 0.1 mass parts, obtains the mixture paste of graphene oxide and elemental sulfur;
Step 3,50 ℃ of heat treatments are after 72 hours in the teflon seal jar with mixture paste, and washing filtering obtains the elemental sulfur composite material of graphitiferous alkene, and wherein the mass content of Graphene is 90%, and the elemental sulfur mass content is 10%.
Embodiment 5
Embodiment 5 is the variant of embodiment 4, is specially:
Step 1 adds the graphene oxide of 1 mass parts in the 100 mass parts deionized waters, makes the dispersion liquid of graphene oxide;
Step 2 adds the elemental sulfur of 30 mass parts, obtains the mixture paste of graphene oxide and elemental sulfur;
Step 3,500 ℃ of heat treatments are after 1 hour in the stainless steel hermetically sealed can with mixture paste, and washing filtering obtains the elemental sulfur composite material of graphitiferous alkene, and wherein the mass content of Graphene is 1%, and the elemental sulfur mass content is 99%.
In the foregoing description, graphene oxide thickness is 0.35～3.5nm, wherein comprises 1～10 graphite flake layer, and said graphite flake layer length and width is respectively 10nm～10 μ m.
In the foregoing description, heat treated is handled in polytetrafluoroethylene that seals or stainless cylinder of steel, carrying out hydro thermal method.
The elemental sulfur composite material of multiple graphitiferous alkene is carried out the SEM test, can see that nano-sulfur particles is dispersed in the surface of Graphene, sees Fig. 1.With the elemental sulfur composite material and the binding agent PTFE of graphitiferous alkene, conductive agent Super P was according to 8: 1: 1 mixed and be made into positive plate; With the lithium metal is negative pole; Cellgard 2400 is a barrier film, and the glycol dimethyl ether of 1mol/L bis trifluoromethyl sulfimide lithium and dioxolane (volume ratio 1: 1) mixed solution are electrolyte, in the argon gas glove box, are assembled into the CR2016 button cell; Carry out the charge-discharge performance test under the room temperature; Specific discharge capacity reaches 1480mAh/g for the second time, and charging and discharging curve is seen Fig. 2, and its cycle performance is seen Fig. 3.
Claims (9)
1. the elemental sulfur composite material of a graphitiferous alkene is characterized in that, said composite material is the binary composite A
xB
y, wherein, A is a Graphene, and B is an elemental sulfur, and B is dispersed in the A surface with the nanometer state, and wherein, x, y are respectively the content of Graphene and elemental sulfur, said 1%≤x≤90%, said 10%≤y≤99%, and x+y=100%.
2. a preparation method who prepares like the elemental sulfur composite material of graphitiferous alkene according to claim 1 is characterized in that, comprises the steps:
Step 1 adds graphene oxide in the deionized water, makes the dispersion liquid of graphene oxide;
Step 2 adds elemental sulfur, obtains the mixture paste of graphene oxide and elemental sulfur;
Step 3, mixture paste carried out heat treated after, washing filtering obtains the elemental sulfur composite material of graphitiferous alkene.
3. the preparation method of the elemental sulfur composite material of graphitiferous alkene according to claim 2; It is characterized in that in step 1, said graphene oxide thickness is 0.35～3.5nm; Wherein comprise 1～10 graphite flake layer, said graphite flake layer length and width is respectively 10nm～10 μ m.
4. the preparation method of the elemental sulfur composite material of graphitiferous alkene according to claim 2 is characterized in that, in step 1, said graphene oxide is 1 mass parts.
5. the preparation method of the elemental sulfur composite material of graphitiferous alkene according to claim 2 is characterized in that, in step 1, said deionized water is the 1-500 mass parts.
6. the preparation method of the elemental sulfur composite material of graphitiferous alkene according to claim 2 is characterized in that, in step 2, said elemental sulfur is the 0.1-30 mass parts.
7. the preparation method of the elemental sulfur composite material of graphitiferous alkene according to claim 2 is characterized in that, in step 3, said heat treated is handled in polytetrafluoroethylene that seals or stainless cylinder of steel, carrying out hydro thermal method.
8. according to the preparation method of the elemental sulfur composite material of claim 2 or 6 described graphitiferous alkene, it is characterized in that in step 3, said heat treated corresponding temperature is 50～500 ℃.
9. the preparation method of the elemental sulfur composite material of graphitiferous alkene according to claim 2 is characterized in that in step 3, and the corresponding time of said heat treated is 1～72 hour.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103682280A (en) * | 2012-09-07 | 2014-03-26 | 中国科学院宁波材料技术与工程研究所 | Lithium-sulfur battery, positive electrode material of battery, and preparation method of material |
| CN103682352A (en) * | 2012-09-07 | 2014-03-26 | 中国科学院宁波材料技术与工程研究所 | Lithium ion secondary battery, positive electrode material of battery, and preparation method of material |
| CN103811731A (en) * | 2012-11-09 | 2014-05-21 | 中国科学院金属研究所 | Graphene-sulfur composite electrode material, preparation method and application thereof |
| CN104300175A (en) * | 2014-10-18 | 2015-01-21 | 山东默锐科技有限公司 | Room-temperature sodium sulfur secondary battery |
| CN104617281A (en) * | 2015-02-12 | 2015-05-13 | 中南大学 | Method for preparing sodium-ion battery antimony/nitrogen-doped carbon nanosheet negative electrode composite material |
| CN105047882A (en) * | 2015-09-09 | 2015-11-11 | 哈尔滨工业大学 | Method for preparing lithium-sulfur battery positive pole material |
| CN105047875A (en) * | 2015-06-25 | 2015-11-11 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of lithium-sulfur battery cathode material |
| CN105355896A (en) * | 2015-10-27 | 2016-02-24 | 上海理工大学 | High-performance lithium-sulfur battery positive electrode material and preparation method therefor |
| CN106848318A (en) * | 2017-01-09 | 2017-06-13 | 迟钝 | A kind of lithium sulfur battery anode material and its preparation method and application |
| CN107452961A (en) * | 2016-05-31 | 2017-12-08 | 罗伯特·博世有限公司 | For lithium-sulfur cell comprising sulfur molecule intercalation in composite positive pole of graphene interlayer structure and preparation method thereof |
| CN107768654A (en) * | 2012-10-26 | 2018-03-06 | 苏州宝时得电动工具有限公司 | The preparation method of electrode composite material, positive pole, the battery with the positive pole |
| CN108258206A (en) * | 2017-12-21 | 2018-07-06 | 肇庆市华师大光电产业研究院 | A kind of positive pole material for high-performance lithium-sulfur battery and preparation method thereof |
| CN111900402A (en) * | 2020-07-29 | 2020-11-06 | 肇庆市华师大光电产业研究院 | Universal electrode material for lithium-sulfur battery and preparation method thereof |
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Cited By (17)
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| CN103682352A (en) * | 2012-09-07 | 2014-03-26 | 中国科学院宁波材料技术与工程研究所 | Lithium ion secondary battery, positive electrode material of battery, and preparation method of material |
| CN103682280A (en) * | 2012-09-07 | 2014-03-26 | 中国科学院宁波材料技术与工程研究所 | Lithium-sulfur battery, positive electrode material of battery, and preparation method of material |
| CN107768654A (en) * | 2012-10-26 | 2018-03-06 | 苏州宝时得电动工具有限公司 | The preparation method of electrode composite material, positive pole, the battery with the positive pole |
| CN103811731A (en) * | 2012-11-09 | 2014-05-21 | 中国科学院金属研究所 | Graphene-sulfur composite electrode material, preparation method and application thereof |
| CN103811731B (en) * | 2012-11-09 | 2016-02-03 | 中国科学院金属研究所 | A kind of graphene-sulfur combination electrode material and its preparation method and application |
| CN104300175B (en) * | 2014-10-18 | 2016-08-17 | 山东默锐科技有限公司 | A kind of room temperature sodium-sulfur secondary battery |
| CN104300175A (en) * | 2014-10-18 | 2015-01-21 | 山东默锐科技有限公司 | Room-temperature sodium sulfur secondary battery |
| CN104617281A (en) * | 2015-02-12 | 2015-05-13 | 中南大学 | Method for preparing sodium-ion battery antimony/nitrogen-doped carbon nanosheet negative electrode composite material |
| CN105047875B (en) * | 2015-06-25 | 2018-01-19 | 中国航空工业集团公司北京航空材料研究院 | A kind of preparation method of lithium sulfur battery anode material |
| CN105047875A (en) * | 2015-06-25 | 2015-11-11 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of lithium-sulfur battery cathode material |
| CN105047882A (en) * | 2015-09-09 | 2015-11-11 | 哈尔滨工业大学 | Method for preparing lithium-sulfur battery positive pole material |
| CN105355896A (en) * | 2015-10-27 | 2016-02-24 | 上海理工大学 | High-performance lithium-sulfur battery positive electrode material and preparation method therefor |
| CN107452961A (en) * | 2016-05-31 | 2017-12-08 | 罗伯特·博世有限公司 | For lithium-sulfur cell comprising sulfur molecule intercalation in composite positive pole of graphene interlayer structure and preparation method thereof |
| CN106848318A (en) * | 2017-01-09 | 2017-06-13 | 迟钝 | A kind of lithium sulfur battery anode material and its preparation method and application |
| CN106848318B (en) * | 2017-01-09 | 2019-06-04 | 迟钝 | A kind of lithium sulfur battery anode material and its preparation method and application |
| CN108258206A (en) * | 2017-12-21 | 2018-07-06 | 肇庆市华师大光电产业研究院 | A kind of positive pole material for high-performance lithium-sulfur battery and preparation method thereof |
| CN111900402A (en) * | 2020-07-29 | 2020-11-06 | 肇庆市华师大光电产业研究院 | Universal electrode material for lithium-sulfur battery and preparation method thereof |
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Application publication date: 20120627 |