CN104900884A - Compressible lithium-sulfur battery electrode material and preparation method thereof - Google Patents
Compressible lithium-sulfur battery electrode material and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
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- H—ELECTRICITY
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- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
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Abstract
The invention relates to a compressible lithium-sulfur battery electrode material and a preparation method thereof. The method employs three-dimensional graphene material with high elasticity as a skeleton for loading elemental sulfur, so as to prepare the composite material with pressure resistance; the material can be uses as a cathode material for compressible lithium-sulfur batteries; and the mass ratio of three-dimensional graphene to elemental sulfur is 1:3-1:7. The preparation method is as below: subjecting a raw material graphene oxide to the processes of hydrothermal reduction and freeze-drying to obtain the three-dimensional graphene material with high elasticity; and compounding with an active material to obtain the composite electrode with high elasticity, which is applicable to compressible lithium-sulfur batteries. The three-dimensional graphene material with high elasticity has the advantages of large surface area, high conductivity and good flexibility, and can be compounded with sulfur to significantly improve the conductivity performance and utilization of sulfur. The compressible composite electrode enables lithium ion battery to stand compression and bending deformation, and is applicable to a variety of wearable lithium-ion batteries.
Description
Technical field
The present invention relates to a kind of preparation method of compressible lithium sulphur battery electrode material, specifically for various wearable lithium-sulfur cell provides the preparation method of the electrode material with high resiliency, compressibility and high stability.
Background technology
Nowadays each electronic product is gradually in microminiaturized high integrated, and various energy storage device arises at the historic moment, and the progress of science and technology impels the requirement of market to battery more and more higher.Lithium secondary battery is a kind of new material battery, and lithium-sulfur cell is wherein acknowledged as 21st century one of energy with development potentiality most.The theoretical specific energy of lithium-sulfur cell can reach 2600Wh/kg, and the theoretical discharge specific discharge capacity of simple substance lithium is 3860mAh/g, and sulphur theoretical discharge specific discharge capacity is 1675mAh/g, much larger than the commercialization secondary cell that present stage uses.In addition, elemental sulfur cheapness, eco-friendly characteristic make again this system great commercial value.But capacity attenuation is fast, cycle performance is poor, the load capacity of sulphur is low and the feature such as poorly conductive governs further developing of lithium-sulfur cell and applies.In order to improve the cyclical stability of lithium-sulfur cell, improve the utilance of active material sulphur, research emphasis in recent years mainly concentrates on sulphur anode composite material aspect.The approach of effective raising lithium-sulfur cell performance finds out a kind of high resiliency, high connductivity and porous material exactly as a matrix, and sulphur content is loose and be fixed on this matrix, forms high performance sulphur anode composite material.
Traditional sulphur anode composite material mainly comprises sulphur/carbon compound, sulphur/polymer compound, sulfur metal compound or sulphur/nanocarbon/metal oxide multiple elements design etc.Although some materials can meet good electric conductivity, the load capacity of sulphur is low, the existence of the problems such as effect of shuttling back and forth, and can not improve the performance of lithium-sulfur cell comprehensively.This just requires to prepare a kind of battery material, there is the loose structure that size is suitable and abundant, active material sulphur high degree of dispersion on base material can be made, internal gutter network can ensure the transmission of ion and electronics, volumetric expansion can be alleviated again and shrink the structure collapses caused in discharge process, thus improve the load capacity of sulphur, ensure the cyclical stability of battery.
In addition, the high resiliency of the preparation of current battery material not lay special stress on material, and along with the development of science and technology, various wearable electronic product arises at the historic moment, in use keep away and unavoidably can produce Tension and Compression, corresponding internal battery is not because have enough pliabilities can deform thereupon yet.Thus, in order to meet the demand of lithium sulfur battery anode material fast development, exploitation one has elastomeric lithium sulfur battery anode material and seems particularly important.
Summary of the invention
Technical problem: the present invention is directed to the demand that wearable electronic needs compressible lithium ion battery, utilize the feature such as high resistance against compression and high resilience of three-dimensional grapheme, by three-dimensional grapheme and sulphur compound, obtain a kind of compressible lithium sulphur battery electrode material and preparation method thereof.
Technical scheme: compressible lithium sulphur battery electrode material employing of the present invention has elastomeric three-dimensional grapheme and obtains the composite material with resistance to pressure as skeleton adulteration elemental sulfur, as the positive electrode of compressible lithium-sulfur cell, wherein the mass ratio of three-dimensional grapheme and sulphur is 1:3 ~ 1:7.
Wherein:
The composite material with resistance to pressure refers under 50% compressed shape variable, removes the material of pressure recovery rate >90%.
The positive electrode of compressible lithium-sulfur cell refers to that pressing down retraction at 50% compressed shape variable answers 1000 times, and the specific capacity of lithium sulfur battery anode material can remain on the material of 900 ~ 1125mAh/g.
Described 50% compressed shape variable refers to that thickness is the compressed shape variable that the composite material of 2cm occurs under the pressure of 100 ~ 1000N.
The preparation method of compressible lithium sulphur battery electrode material of the present invention comprises:
1) Hydrothermal Synthesis: graphene oxide is placed in hydrothermal reaction kettle and carries out the three-dimensional grapheme hydrogel material that hydro-thermal reaction obtains self assembly, hydrothermal temperature is 150 ~ 200 degrees Celsius, and the hydro-thermal reaction time is 8 ~ 12 hours;
2) freeze drying, cutting processing: the three-dimensional grapheme hydrogel of the self assembly of acquisition is put into freeze drier and carries out freeze drying process, the vacuum degree of freeze drying process is 0.1 ~ 10torr, time is 12 ~ 48 hours, acquisition has loose structure, resistance against compression and elastomeric three-dimensional grapheme material, is cut into the three-dimensional grapheme flaky material of thickness 0.5 ~ 5cm with freezing-microtome;
3) melting distillation: elemental sulfur powder is sprinkled upon uniformly on the three-dimensional grapheme flaky material of well cutting, again the mixture of elemental sulfur powder and three-dimensional grapheme flaky material is put into vacuum drying chamber sulphur melting to be distilled be coated on graphene sheet layer, namely obtain the compressible lithium sulphur battery electrode material of three-dimensional graphite thiazolinyl.
By above step, the loose structure structural stability of the three-dimensional grapheme of acquisition is strong, the pliability making it good and resilience, and material can keep three-dimensional structure to stablize by compression, and Quick-return original appearance after pressure removal.The loose structure of obtained carbon nanomaterial makes the load capacity of sulphur greatly improve, and inhibits effect of shuttling back and forth, further increases chemical property and the energy-storage property of lithium-sulfur cell.Test through battery performance and mechanical performance finds, carries out compression combined electrode with 50% deformation quantity, circulate still can keep for 1000 times 90% response rate, and the specific capacity of combination electrode remains on 910 ~ 1125mAh/g.
Beneficial effect: carbon nanomaterial of the present invention is all cheap, simple and easy to get, without the need to harsh conditions such as HTHPs in preparation technology, is easy to makely suitable for large-scale production industrialization.Hydrothermal reduction method in the present invention, freeze drying, cutting processing, melting distillation all can effectively complete, and can obtain the lithium sulfur battery anode material with resistance against compression and good electrical chemical property.The compression resistant lithium ion battery of the preparation-obtained three-dimensional grapheme combination electrode material assembling of the present invention shows through measuring mechanical property, so that the response rate of more than 90% still can be kept after 50% deformation quantity compression reaction 1000 times, and its capacity can remain in the scope of 910 ~ 1125mAh/g, the shape breaching battery by compression with the limitation of stretcher strain, for the making of the Wearable electronic product that variously to stretch, compress or equipment internal battery material provides solution.
Embodiment
The preparation method of compressible lithium sulphur battery electrode of the present invention comprises the following steps:
1) hydro-thermal synthesis process: graphene oxide is placed in hydrothermal reaction kettle and carries out the three-dimensional grapheme material that hydro-thermal reaction obtains self assembly, hydrothermal temperature is 150 ~ 200 degrees Celsius, and the hydro-thermal reaction time is 8 ~ 12 hours;
2) freeze drying, cutting processing: the three-dimensional grapheme hydrogel of the self assembly of acquisition is put into freeze drier and carries out freeze drying process, the vacuum degree of freeze drying process is 0.1 ~ 10torr, time is 12 ~ 48 hours, acquisition has loose structure, resistance against compression and elastomeric three-dimensional grapheme material, is cut into the flaky material of 2cm thickness with freezing-microtome;
3) melting distillation: elemental sulfur powder is sprinkled upon on the three-dimensional grapheme flaky material of well cutting uniformly.Mixture being put into vacuum drying chamber makes sulphur melting distillation be coated on graphene sheet layer, namely obtains the compressible combination electrode material of three-dimensional graphite thiazolinyl.
Below by embodiment, the present invention is set forth through row, but do not limit the present invention.
Embodiment 1
Selection caliber is 20nm, and length is the carbon nano-tube of 10 μm, is hybridly prepared into graphene oxide/carbon nano-tube aqueous solutions by after its acidification with the graphene oxide solution of 2mol/ml, and wherein the mass ratio of graphene oxide and carbon nano-tube is 1:3.Poured into by mixed solution in the hydrothermal reaction kettle of tetrafluoroethene liner and carry out hydro-thermal reaction, hydrothermal temperature is 155 DEG C, and the hydro-thermal reaction time is 10 hours, obtains the three-dimensional grapheme hydrogel of self assembly after reaction terminates.Put it into freeze drying in freeze drier subsequently and after 24 hours, just obtain the three-dimensional grapheme of porous high-elastic.With slicing machine, three-dimensional grapheme is cut into the thin slice that thickness is 2cm, sulphur powder is spilt at its surface uniform, wherein the mass ratio of three-dimensional grapheme and sulphur powder is 1:5, and under the condition of 155 DEG C, reaction can obtain the lithium sulfur battery anode material of high resiliency three-dimensional graphite base for 10 hours.Battery performance and measuring mechanical property display are with 50% deformation quantity compression reaction 1000 times, and its specific capacity remains on 1013mAh/g.
Embodiment 2
Selection caliber is 20nm, and length is the carbon nano-tube of 10 μm, is hybridly prepared into graphene oxide/carbon nano-tube aqueous solutions by after its acidification with the graphene oxide solution of 2mol/ml, and wherein the mass ratio of graphene oxide and carbon nano-tube is 1:5.Poured into by mixed solution in the hydrothermal reaction kettle of tetrafluoroethene liner and carry out hydro-thermal reaction, hydrothermal temperature is 155 DEG C, and the hydro-thermal reaction time is 10 hours, obtains the three-dimensional grapheme hydrogel of self assembly after reaction terminates.Put it into freeze drying in freeze drier subsequently and after 24 hours, just obtain the three-dimensional grapheme of porous high-elastic.With slicing machine, three-dimensional grapheme is cut into the thin slice that thickness is 2cm, sulphur powder is spilt at its surface uniform, wherein the mass ratio of three-dimensional grapheme and sulphur powder is 1:5, and under the condition of 155 DEG C, reaction can obtain the lithium sulfur battery anode material of high resiliency three-dimensional graphite base for 10 hours.Battery performance and measuring mechanical property display are with 50% deformation quantity compression reaction 1000 times, and its specific capacity remains on 931mAh/g.
Embodiment 3
Selection caliber is 20nm, and length is the carbon nano-tube of 10 μm, is hybridly prepared into graphene oxide/carbon nano-tube aqueous solutions by after its acidification with the graphene oxide solution of 2mol/ml, and wherein the mass ratio of graphene oxide and carbon nano-tube is 1:5.Poured into by mixed solution in the hydrothermal reaction kettle of tetrafluoroethene liner and carry out hydro-thermal reaction, hydrothermal temperature is 155 DEG C, and the hydro-thermal reaction time is 10 hours, obtains the three-dimensional grapheme hydrogel of self assembly after reaction terminates.Put it into freeze drying in freeze drier subsequently and after 24 hours, just obtain the three-dimensional grapheme of porous high-elastic.With slicing machine, three-dimensional grapheme is cut into the thin slice that thickness is 2cm, sulphur powder is spilt at its surface uniform, wherein the mass ratio of three-dimensional grapheme and sulphur powder is 1:3, and under the condition of 155 DEG C, reaction can obtain the lithium sulfur battery anode material of high resiliency three-dimensional graphite base for 10 hours.Battery performance and measuring mechanical property display are with 50% deformation quantity compression reaction 1000 times, and its specific capacity remains on 996mAh/g.
Embodiment 4
Selection caliber is 20nm, and length is the carbon nano-tube of 10 μm, is hybridly prepared into graphene oxide/carbon nano-tube aqueous solutions by after its acidification with the graphene oxide solution of 2mol/ml, and wherein the mass ratio of graphene oxide and carbon nano-tube is 1:3.Poured into by mixed solution in the hydrothermal reaction kettle of tetrafluoroethene liner and carry out hydro-thermal reaction, hydrothermal temperature is 155 DEG C, and the hydro-thermal reaction time is 10 hours, obtains the three-dimensional grapheme hydrogel of self assembly after reaction terminates.Put it into freeze drying in freeze drier subsequently and after 24 hours, just obtain the three-dimensional grapheme of porous high-elastic.With slicing machine, three-dimensional grapheme is cut into the thin slice that thickness is 2cm, sulphur powder is spilt at its surface uniform, wherein the mass ratio of three-dimensional grapheme and sulphur powder is 1:7, and under the condition of 155 DEG C, reaction can obtain the lithium sulfur battery anode material of high resiliency three-dimensional graphite base for 10 hours.Battery performance and measuring mechanical property display are with 50% deformation quantity compression reaction 1000 times, and its specific capacity remains on 1125mAh/g.
Embodiment 5
Select the graphene oxide solution of 2mol/ml, poured into by solution in the hydrothermal reaction kettle of tetrafluoroethene liner and carry out hydro-thermal reaction, hydrothermal temperature is 155 DEG C, and the hydro-thermal reaction time is 10 hours, obtains the three-dimensional grapheme hydrogel of self assembly after reaction terminates.Put it into freeze drying in freeze drier subsequently and after 24 hours, just obtain the three-dimensional grapheme of porous high-elastic.With slicing machine, three-dimensional grapheme is cut into the thin slice that thickness is 2cm, sulphur powder is spilt at its surface uniform, wherein the mass ratio of three-dimensional grapheme and sulphur powder is 1:3, and under the condition of 155 DEG C, reaction can obtain the lithium sulfur battery anode material of high resiliency three-dimensional graphite base for 10 hours.Battery performance and measuring mechanical property display are with 50% deformation quantity compression reaction 1000 times, and its specific capacity remains on 998mAh/g.
Embodiment 6
Select the graphene oxide solution of 2mol/ml, poured into by solution in the hydrothermal reaction kettle of tetrafluoroethene liner and carry out hydro-thermal reaction, hydrothermal temperature is 155 DEG C, and the hydro-thermal reaction time is 10 hours, obtains the three-dimensional grapheme hydrogel of self assembly after reaction terminates.Put it into freeze drying in freeze drier subsequently and after 24 hours, just obtain the three-dimensional grapheme of porous high-elastic.With slicing machine, three-dimensional grapheme is cut into the thin slice that thickness is 2cm, sulphur powder is spilt at its surface uniform, wherein the mass ratio of three-dimensional grapheme and sulphur powder is 1:5, and under the condition of 155 DEG C, reaction can obtain the lithium sulfur battery anode material of high resiliency three-dimensional graphite base for 10 hours.Battery performance and measuring mechanical property display are with 50% deformation quantity compression reaction 1000 times, and its specific capacity remains on 1020mAh/g.
Claims (5)
1. a compressible lithium sulphur battery electrode material, it is characterized in that: the employing of this material has elastomeric three-dimensional grapheme and obtains the composite material with resistance to pressure as skeleton adulteration elemental sulfur, as the positive electrode of compressible lithium-sulfur cell, wherein the mass ratio of three-dimensional grapheme and sulphur is 1:3 ~ 1:7.
2. compressible lithium sulphur battery electrode material according to claim 1, is characterized in that: the composite material with resistance to pressure refers under 50% compressed shape variable, removes the material of pressure recovery rate >90%.
3. compressible lithium sulphur battery electrode material according to claim 1, it is characterized in that: the positive electrode of compressible lithium-sulfur cell refers to that pressing down retraction at 50% compressed shape variable answers 1000 times, and the specific capacity of lithium sulfur battery anode material can remain on the material of 900 ~ 1125mAh/g.
4. compressible lithium sulphur battery electrode material according to claim 3, is characterized in that: described 50% compressed shape variable refers to that thickness is the compressed shape variable that the composite material of 2cm occurs under the pressure of 100 ~ 1000N.
5. a preparation method for compressible lithium sulphur battery electrode material as claimed in claim 1, is characterized in that the method comprises:
1) Hydrothermal Synthesis: graphene oxide is placed in hydrothermal reaction kettle and carries out the three-dimensional grapheme hydrogel material that hydro-thermal reaction obtains self assembly, hydrothermal temperature is 150 ~ 200 DEG C, and the hydro-thermal reaction time is 8 ~ 12 hours;
2) freeze drying, cutting processing: the three-dimensional grapheme hydrogel of the self assembly of acquisition is put into freeze drier and carries out freeze drying process, the vacuum degree of freeze drying process is 0.1 ~ 10torr, time is 12 ~ 48 hours, acquisition has loose structure, resistance against compression and elastomeric three-dimensional grapheme material, is cut into the three-dimensional grapheme flaky material of thickness 0.5 ~ 5cm with freezing-microtome;
3) melting distillation: elemental sulfur powder is sprinkled upon uniformly on the three-dimensional grapheme flaky material of well cutting, again the mixture of elemental sulfur powder and three-dimensional grapheme flaky material is put into vacuum drying chamber sulphur melting to be distilled be coated on graphene sheet layer, namely obtain the compressible lithium sulphur battery electrode material of three-dimensional graphite thiazolinyl.
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Cited By (7)
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| CN106384828A (en) * | 2016-10-19 | 2017-02-08 | 天津力神电池股份有限公司 | Crosslinking porous composite lithium-sulfur battery anode and preparation method thereof |
| CN106410116A (en) * | 2016-10-19 | 2017-02-15 | 天津力神电池股份有限公司 | Graded porous composite lithium-sulfur battery cathode 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 |
| WO2021047354A1 (en) * | 2019-09-12 | 2021-03-18 | 齐鲁工业大学 | Pine branch-shaped samarium oxide-graphene-sulfur gel structure material, preparation method therefor, and application thereof |
| CN113493199A (en) * | 2020-03-19 | 2021-10-12 | 中国科学院上海硅酸盐研究所 | Preparation method of high-conductivity and high-elasticity three-dimensional graphene material |
| CN114843464A (en) * | 2022-04-21 | 2022-08-02 | 陕西科技大学 | Three-dimensional cross-linked structure SnSe/3D r-GO composite material and preparation method and application thereof |
| WO2023246795A1 (en) * | 2022-06-21 | 2023-12-28 | 比亚迪股份有限公司 | Negative electrode sheet, secondary battery, and electric device |
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| WO2021047354A1 (en) * | 2019-09-12 | 2021-03-18 | 齐鲁工业大学 | Pine branch-shaped samarium oxide-graphene-sulfur gel structure material, preparation method therefor, and application thereof |
| CN113493199A (en) * | 2020-03-19 | 2021-10-12 | 中国科学院上海硅酸盐研究所 | Preparation method of high-conductivity and high-elasticity three-dimensional graphene material |
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Application publication date: 20150909 |