CN107017392A - A kind of preparation method of sodium-ion battery metal sulfide/graphene - Google Patents
A kind of preparation method of sodium-ion battery metal sulfide/graphene Download PDFInfo
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- CN107017392A CN107017392A CN201710305997.5A CN201710305997A CN107017392A CN 107017392 A CN107017392 A CN 107017392A CN 201710305997 A CN201710305997 A CN 201710305997A CN 107017392 A CN107017392 A CN 107017392A
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- preparation
- methylimidazoles
- ion battery
- atmosphere
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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
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 method of sodium-ion battery metal sulfide/graphene; graphite oxide is added in ionic liquid; ultrasonic disperse, obtains GO dispersion liquids, and source metal is added in GO dispersion liquids; stirring mixing; sulphur source is added, ion thermal response is carried out, obtained material is washed after drying; calcined in tube furnace under inert atmosphere protection, obtain metal sulfide/graphene composite material.The method that the present invention is provided is simple, solvent and structure directing agent are used as using ionic liquid, prepare metal sulfide/graphene composite material with high conductivity and satisfactory texture stability, and apply it in sodium-ion battery, higher capacity is obtained, the design preparation for sodium ion battery electrode material has great importance.
Description
Technical field
The present invention relates to a kind of preparation method of sodium-ion battery metal sulfide/graphene, technique is simple, and green is without dirt
Dye, degree of being practical is high, and obtained sulfide/graphene can be directly as anode material of lithium-ion battery.
Background technology
Lithium rechargeable battery is as one of energy storage device in portable type electronic product, electric tool and electric automobile field
Developed rapidly, social fast development also make it that people are increasing to the demand of lithium ion battery, therefore also to lithium
The performance requirement more and more higher of ion battery, should ensure good security and cyclical stability, meet touched in big rule again
Using when especially in high current charge-discharge with good high rate performance.But the distribution of lithium resource on earth and inequality
It is even, and the price of lithium rises, and raises lithium ion battery cost.And the sodium and lithium for being in same main group with lithium have phase
As physicochemical property, and sodium aboundresources is widely distributed, and price is than relatively low, and therefore, the cost of material of sodium-ion battery is far low
In the material of lithium ion battery.In summary, exploitation sodium-ion battery is to non-as the potential additional project of lithium ion battery
Chang Heli and great feasibility, thus receive the extensive concern of people.
Metal sulfide (Sb2S3, Bi2S3, SnS etc.) as anode material of lithium-ion battery when, converted before this with sodium
Reaction, generates metal simple-substance, and then occurs alloying reaction, therefore can shift more electronics, with higher theory
Specific capacity, and with the invertibity higher relative to oxide, therefore research sulfide has certain meaning.However, should
When class material is as anode material of lithium-ion battery, on the one hand with relatively low electric conductivity, on the other hand, it is in charge and discharge process
Middle Volume Changes are larger, and structure is easily destroyed, and causes cycle performance poor.For this problem, people have done some to it
Research, research is found, metal sulfide and carbon material are combined, the high conductivity and loose structure of carbon material, Ke Yihuan is utilized
Solve some problems present in this kind of material.
Ion thermal synthesis method refers to replace conventional water or organic solvent work with ionic liquid (including eutectic mixture)
For the material synthesis method of reaction medium.Ionic liquid by organic cation and anion constitute room temperature or it is near at room temperature
For the salt of liquid, with non-volatile, free of contamination characteristic, therefore it is referred to as green solvent.Yin Qigao heat, chemical stability,
The advantages of structure designability, is gradually paid close attention in material preparation by people.Due to alternative ionic liquid species and
Number is various, therefore using different types of ionic liquid is possible to synthesize the material of different structure.With to ionic liquid
The continuous development of the research of body, prepares material as solvent and has also obtained more research, and show unique advantage.
The content of the invention
The purpose of the present invention be for sulfide as some problems present in anode material of lithium-ion battery there is provided
A kind of preparation method of metal sulfide/graphene composite material, the present invention prepares metal by simple ion thermal method
Sulfide/graphene composite material, and anode material of lithium-ion battery is applied it to, fully combine the Fabrication of High Specific Capacitance of sulfide
Amount, the high conductivity of graphene, high-specific surface area prepare capacity height, the high composite of coulombic efficiency.
Technical scheme:
A kind of preparation method of sodium-ion battery metal sulfide/graphene, step is as follows:
Graphite oxide is scattered in ionic liquid, ultrasonic disperse, obtains GO dispersion liquids, source metal is added into GO disperses
In liquid, continue ultrasound and obtain precursor liquid.Sulphur source is added in precursor liquid, the solution is heated, the reaction time is 8-20h, is washed
Wash and calcined after drying in tube furnace under inert atmosphere protection, obtain metal sulfide/graphene composite material.
Described graphite oxide is prepared by amended Hummers, and the concentration of GO dispersion liquids is 1mgml-1~
12mg·ml-1。
Described ionic liquid is 1- butyl -3- methylimidazolium hydrogen sulphate salt (BMIMHSO4), 1- pi-allyl -3- methyl miaows
Azoles disulfate (AMIMHSO4), 1- ethyl-3-methylimidazole disulfates (EMIMHSO4), 1- propyl group -3- methylimidazole sulfuric acid
Hydrogen salt (PMIMHSO4), 1- butyl -3- methylimidazole dihydric phosphates (BMIMH2PO4), 1- pi-allyl -3- methylimidazole phosphoric acid
Dihydric salt (AMIM H2PO4), 1- ethyl-3-methylimidazole dihydric phosphates (EMIMH2PO4), 1- propyl group -3- methylimidazole phosphorus
Acid dihydride salt (PMIMH2PO4), 1- butyl -3- methylimidazole bisulfites (BMIMHSO3), 1- pi-allyl -3- methylimidazoles
Bisulfites (AMIMHSO3), 1- ethyl-3-methylimidazole bisulfites (EMIMHSO3), 1- propyl group -3- methylimidazoles it is sub-
Disulfate (PMIMHSO3), 1- butyl -3- methyl imidazolium tetrafluoroborates (BMIMBF4), 1- pi-allyl -3- methylimidazoles four
Borofluoride (AMIMBF4), 1- ethyl-3-methylimidazole tetrafluoroborates (EMIMBF4), 1- propyl group -3- methylimidazole tetrafluoro boron
Hydrochlorate (PMIMBF4) one or both of it is mixed above;It is preferred that 1- butyl -3- methylimidazole dihydric phosphates (BMIMH2PO4)
With 1- pi-allyl -3- methylimidazole dihydric phosphates (AMIMH2PO4)。
Described source metal is SbCl3、BiCl3、SnCl2·2H2O、SnCl4·5H2O、Na2MoO4·2H2O.、CoCl2·
6H2O、Zn(Ac)2·2H2O、FeCl3·6H2O、Ni(NO3)2·6H2O、(CH3COO)2Cu·H2O、ZnCl2、(CH3COO)2Cd·2H2The mass ratio of O, source metal and graphite oxide is 4:1~10:1.
Described sulphur source is thioacetamide, thiocarbamide, Na2S, sulphur powder, Cys, L-cysteine hydrochloride,
Na2S2O3。
Described ultrasonic disperse ultrasonic cleaner, Parameter Conditions are:20-40 DEG C, ultrasonic 1-4h.
Described heating-up temperature is 150-220 DEG C, and the reaction time is 8-20h.
Described inert atmosphere is N2Atmosphere or Ar atmosphere.
Described calcining heat is 350-550 DEG C, and the time is 3-6h.
The preparation method has prepared metal sulfide/graphene composite material using ionic liquid as solvent, and by its
Applied to sodium-ion battery negative pole.
Beneficial effects of the present invention:This method is using ionic liquid as solvent, while as template and structure directing agent,
The compound firm, product of metal sulfide/graphene composite material of preparation is uniform, and is used as anode material of lithium-ion battery
Capacity is high.This method is simple, and raw material is easy to get, environmental protection.Design for sodium ion battery electrode material is prepared with important
Meaning.
Brief description of the drawings
Fig. 1 is Sb prepared by embodiment 12S3The SEM figures of/graphene composite material.Sb as seen from the figure2S3Equably
It is dispersed in graphene, and does not lump.
Fig. 2 is Sb prepared by embodiment 12S3The XRD of/graphene composite material.As can be seen that using ionic liquid to be molten
Agent, what is obtained is the Sb of crystal structure2S3。
Fig. 3 is Sb prepared by embodiment 12S3/ graphene composite material is 50mAg in current density-1Under it is preceding twice
Charging and discharging curve figure.
Fig. 4 is Sb prepared by embodiment 12S3The high rate performance figure of/graphene composite material.
Embodiment
Below in conjunction with accompanying drawing and technical scheme, the embodiment of the present invention is further illustrated.
Embodiment 1:
40mg graphene oxides are added to 5ml BMIMH2PO4In, ultrasound 3h, obtains the ion of graphite oxide at 30 DEG C
Liquid dispersion, adds 0.25gSbCl3, ultrasonic 2h treats SbCl3It is scattered in after graphite oxide dispersion, adds 0.2g thio
Acetamide, 12h is reacted at 180 DEG C, after washing is dried, presoma is obtained, by the presoma 500 DEG C of burnings under an argon atmosphere
3h, obtains Sb2S3/ graphene composite material.
Embodiment 2:
40mg graphene oxides are added to 5ml BMIMH2PO4In, ultrasound 3h, the ionic liquid aoxidized at 30 DEG C
Dispersion liquid, adds 0.25gBiCl3, ultrasonic 2h treats BiCl3It is scattered in after graphite oxide dispersion, adds 0.2g thioacetyls
Amine, 12h is reacted at 180 DEG C, after washing is dried, presoma is obtained, and the presoma 550 DEG C of burning 3h under an argon atmosphere are obtained
To Sb2S3/ graphene composite material.
Embodiment 3:
50mg graphene oxides are added to 5ml BMIMHSO4In, ultrasound 3h, obtains the ion of graphite oxide at 30 DEG C
Liquid dispersion, adds 0.25gSbCl3, ultrasonic 2h treats SbCl3It is scattered in after graphite oxide dispersion, adds 0.2g thiocarbamides,
12h is reacted at 180 DEG C, after washing is dried, presoma is obtained, the presoma is burnt into 3h for 500 DEG C under an argon atmosphere, obtained
Sb2S3/ graphene composite material.
Embodiment 4:
50mg graphene oxides are added to 5ml BMIMH2PO4In, ultrasound 3h, obtains the ion of graphite oxide at 30 DEG C
Liquid dispersion, adds 0.25gSnCl2·2H2O, ultrasonic 2h, treats SnCl2·2H2O is scattered in after graphite oxide dispersion, then
Add and 20h is reacted at 0.1g thioacetamides, 180 DEG C, after washing is dried, presoma is obtained, by the presoma in argon gas gas
The lower 500 DEG C of burnings 3h of atmosphere, obtains SnS/ graphene composite materials.
Claims (10)
1. a kind of preparation method of sodium-ion battery metal sulfide/graphene, it is characterised in that step is as follows:Stone will be aoxidized
Ink is scattered in ionic liquid, ultrasonic disperse, obtains GO dispersion liquids;Source metal is added in GO dispersion liquids, continues ultrasound, obtains
To precursor liquid;Sulphur source is added in precursor liquid, 150-220 DEG C of temperature conditionss lower reaction time is 8-20h, after washing is dried,
Calcined in tube furnace under inert atmosphere protection, calcining heat is 350-550 DEG C, and the time is 3-6h, obtain sodium-ion battery gold
Belong to sulfide/graphene;
Wherein, the concentration of GO dispersion liquids is 1mgml-1~12mgml-1;
The mass ratio of source metal and graphite oxide is 4:1~10:1.
2. preparation method according to claim 1, it is characterised in that the ionic liquid is 1- butyl -3- methylimidazoles
Disulfate, 1- pi-allyl -3- methylimidazolium hydrogen sulphates salt, 1- ethyl-3-methylimidazoles disulfate, 1- propyl group -3- methyl
Imidazole bisulfate, 1- butyl -3- methylimidazoles dihydric phosphate, 1- pi-allyl -3- methylimidazoles dihydric phosphate, 1- second
Base -3- methylimidazoles dihydric phosphate, 1- propyl group -3- methylimidazoles dihydric phosphate, 1- butyl -3- methylimidazole bisulfites
Salt, 1- pi-allyl -3- methylimidazoles bisulfites, 1- ethyl-3-methylimidazoles bisulfites, 1- propyl group -3- methyl miaows
Azoles bisulfites, 1- butyl -3- methyl imidazolium tetrafluoroborates, 1- pi-allyl -3- methyl imidazolium tetrafluoroborates, 1- second
One or both of base -3- methyl imidazolium tetrafluoroborates, 1- propyl group -3- methyl imidazolium tetrafluoroborates are mixed above.
3. preparation method according to claim 1 or 2, it is characterised in that described source metal is SbCl3、BiCl3、
SnCl2·2H2O、SnCl4·5H2O、Na2MoO4·2H2O、CoCl2·6H2O、Zn(Ac)2·2H2O、FeCl3·6H2O、Ni
(NO3)2·6H2O、(CH3COO)2Cu·H2O、ZnCl2、(CH3COO)2Cd·2H2One or both of O is mixed above.
4. preparation method according to claim 1 or 2, it is characterised in that described sulphur source be thioacetamide, thiocarbamide,
Na2S, sulphur powder, Cys, L-cysteine hydrochloride or Na2S2O3。
5. preparation method according to claim 3, it is characterised in that described sulphur source is thioacetamide, thiocarbamide, Na2S、
Sulphur powder, Cys, L-cysteine hydrochloride or Na2S2O3。
6. the preparation method according to claim 1,2 or 5, it is characterised in that described inert atmosphere is N2Atmosphere or Ar gas
Atmosphere.
7. preparation method according to claim 3, it is characterised in that described inert atmosphere is N2Atmosphere or Ar atmosphere.
8. preparation method according to claim 4, it is characterised in that described inert atmosphere is N2Atmosphere or Ar atmosphere.
9. the preparation method according to claim 1,2,5,7 or 8, it is characterised in that described ultrasonic disperse is at 20-40 DEG C
Ultrasound 1-4h under temperature conditionss;Described graphite oxide is prepared by amended Hummers.
10. preparation method according to claim 6, it is characterised in that described ultrasonic disperse is in 20-40 DEG C of temperature conditionss
Lower ultrasonic 1-4h;Described graphite oxide is prepared by amended Hummers.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109659544A (en) * | 2018-12-24 | 2019-04-19 | 肇庆市华师大光电产业研究院 | A kind of lithium/anode material of lithium-ion battery preparation method of graphene coated bimetallic sulfide |
CN111704138A (en) * | 2020-06-03 | 2020-09-25 | 大连理工大学 | Preparation method of two-dimensional nanocomposite material self-assembled layer by layer |
CN111916707A (en) * | 2020-08-12 | 2020-11-10 | 陕西师范大学 | Preparation method and application of graphene @ molybdenum diselenide @ SnS heterogeneous interface composite material |
CN112289978A (en) * | 2020-06-03 | 2021-01-29 | 大连理工大学 | Composite lithium metal negative electrode and preparation method thereof |
CN113346058A (en) * | 2021-05-21 | 2021-09-03 | 大连理工大学 | Method for preparing bimetallic sulfide and carbon compound under ionic gel system |
CN113346058B (en) * | 2021-05-21 | 2024-05-17 | 大连理工大学 | Method for preparing bimetallic sulfide and carbon composite under ion gel system |
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CN104843682A (en) * | 2015-04-07 | 2015-08-19 | 大连理工大学 | Preparation method and application of reduced graphene oxide |
CN105161691A (en) * | 2015-10-10 | 2015-12-16 | 岭南师范学院 | Preparation method of less-layer MoS2/phosphorus-doped graphene electrochemical sodium-storage combined electrode |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN109659544A (en) * | 2018-12-24 | 2019-04-19 | 肇庆市华师大光电产业研究院 | A kind of lithium/anode material of lithium-ion battery preparation method of graphene coated bimetallic sulfide |
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CN112289978A (en) * | 2020-06-03 | 2021-01-29 | 大连理工大学 | Composite lithium metal negative electrode and preparation method thereof |
CN112289978B (en) * | 2020-06-03 | 2022-04-08 | 大连理工大学 | Composite lithium metal negative electrode and preparation method thereof |
CN111916707A (en) * | 2020-08-12 | 2020-11-10 | 陕西师范大学 | Preparation method and application of graphene @ molybdenum diselenide @ SnS heterogeneous interface composite material |
CN111916707B (en) * | 2020-08-12 | 2021-07-16 | 陕西师范大学 | Preparation method and application of graphene @ molybdenum diselenide @ SnS heterogeneous interface composite material |
CN113346058A (en) * | 2021-05-21 | 2021-09-03 | 大连理工大学 | Method for preparing bimetallic sulfide and carbon compound under ionic gel system |
CN113346058B (en) * | 2021-05-21 | 2024-05-17 | 大连理工大学 | Method for preparing bimetallic sulfide and carbon composite under ion gel system |
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