CN110112374A - A kind of phosphorus doping graphene carbon fiber Ryukyu aeroge and the preparation method and application thereof - Google Patents
A kind of phosphorus doping graphene carbon fiber Ryukyu aeroge and the preparation method and application thereof Download PDFInfo
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- CN110112374A CN110112374A CN201910198511.1A CN201910198511A CN110112374A CN 110112374 A CN110112374 A CN 110112374A CN 201910198511 A CN201910198511 A CN 201910198511A CN 110112374 A CN110112374 A CN 110112374A
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- carbon fiber
- aeroge
- ryukyu
- phosphorus doping
- sulphur
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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
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
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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
A kind of phosphorus doping graphene carbon fiber Ryukyu aeroge and the preparation method and application thereof, is related to lithium sulphur battery electrode technical field, and preparation method includes preparing carbon fiber respectively and obtaining Ryukyu；In the graphene oxide solution that Ryukyu is dispersed in, carbon fiber is added, is uniformly mixed, is freeze-dried to obtain graphene oxide/carbon fiber/sulphur aeroge；Graphene oxide/carbon fiber/sulphur aeroge is added phosphoric acid solution and is placed in water heating kettle and is reacted, hydrazine hydrate reduction obtains phosphorus doping graphene carbon fiber Ryukyu aeroge.The carbon-based Ryukyu's carbon fiber aerogel material of phosphorus doping prepared by the present invention, carbon fiber is connected to the structure of reinforcing material between graphene and increases the electric conductivity of material, duct in aeroge is provided sufficient space by the volume expansion that sulphur anode occurs in charge and discharge process, material structure is set to keep stablizing during battery cycle charge-discharge, the service life for extending material improves the cyclical stability of battery.
Description
Technical field
The present invention relates to lithium sulphur battery electrode technical fields, and in particular to a kind of phosphorus doping graphene carbon fiber Ryukyu's airsetting
Glue and the preparation method and application thereof.
Background technique
In numerous electrochemical energy storage systems, lithium-sulfur cell is considered as a kind of secondary lithium of new generation of great development prospect
Battery.Lithium-sulfur cell has high theoretical capacity (~1675mAh/g) and high-energy density (~2600Wh/kg).Moreover,
Elemental sulfur as a positive electrode active material has a rich reserves, from a wealth of sources and less toxic nuisanceless equal many merits, therefore, largely
Researchers be devoted in the research of lithium-sulfur cell commercial applications.
Although the application prospect of lithium-sulfur cell is very bright, lithium-sulfur cell at this stage commercialization still by
It is hindered to some problems not yet overcome, such as: (1) more lithium sulfides that battery is formed during the charging process are between positive and negative anodes
Reciprocating motion forms shuttle effect, this phenomenon causes battery charging process to extend, and coulombic efficiency reduces, and more lithium sulfides corrode
Cathode of lithium consumes the content of lithium, while more lithium sulfides of cathode are reduced to nonconducting Li2S2And Li2S is deposited on lithium piece
Surface hinders electron-transport to also result in active material loss, reduces the cycle performance of battery；(2) sulphur is as positive electrode active material
Matter, conductivity is lower, and the essence of insulation hinders the transmission of electronics in electrode, and the utilization rate of active material is caused to reduce；(3)
Battery mutually converting there are sulphur and more lithium sulfides in charge and discharge process, the swollen of volume can also occur for the electrode structure of sulphur anode
Swollen and shrinkage phenomenon, volume expansion and contraction repeatedly will cause electrode structure and collapse and active material the problems such as falling off, thus
Reduce the volumetric properties of battery.
Currently, people improve these problems of lithium-sulfur cell by a variety of methods, and such as: it is (more that sulphur is loaded to carbon material
Hole carbon ball, mesoporous carbon fiber, carbon nanotube, graphene etc.), porous metal oxide etc..Such as: sulphur is loaded to mesoporous carbon
CMK-3 and positive electrode as lithium-sulfur cell, the specific capacity of the battery can achieve 1051mAh/g, and maintain following for 200 circles
Ring stability.Sulphur is loaded in the nucleocapsid carbon ball with hollow structure and is prepared into solid carbon ball/sulphur composite material, which makees
The specific capacity of 960mAh/g is still maintained after the circle of circulation 200 for lithium-sulphur cell positive electrode.But existing porous lithium-sulfur cell
The limited load sulfur content for leading to material of the pore volume of positive electrode is lower, to limit the chemical property of battery.
Summary of the invention
It is high that the object of the present invention is to provide a kind of sulfur contents, and active utilization rate is high, and energy density is high, and good cycle is just
Pole material and preparation method thereof, to overcome sulphur loading existing for existing sulphur positive electrode low, specific capacity is small, energy density
It is low, the problems such as poor circulation.
For achieving the above object, technical scheme is as follows:
A kind of preparation method of phosphorus doping graphene carbon fiber Ryukyu aeroge comprising following steps:
S1: being made polyimide film for polyimide solution, and carbonization is heated in protective atmosphere, obtains carbon-fiber film, then by carbon
Tunica fibrosa immerses the concentrated sulfuric acid, and ultrasound is washed, dry, obtains carbon fiber；
By Na2S2O3Solution is mixed with polyvinylpyrrolidone, and concentrated hydrochloric acid is added, and is stirred, filtering, and deionized water washing obtains
Ryukyu；
S2: in the graphene oxide solution that the Ryukyu prepared in S1 is dispersed in, the carbon fiber prepared in S1, mixing is added
Uniformly, it is freeze-dried to obtain graphene oxide/carbon fiber/sulphur aeroge；
S3: phosphoric acid solution is added in graphene oxide/carbon fiber/sulphur aeroge, is placed in water heating kettle and reacts, filters, washes
It washs, it is dry, obtain phosphorus doping graphene oxide carbon fiber/sulphur aeroge；
S4: by phosphorus doping graphene oxide carbon fiber/sulphur ball aeroge hydrazine hydrate reduction, phosphorus doping graphene carbon fiber is obtained
Tie up Ryukyu's aeroge.
Technical solution as a further improvement of that present invention, the step S1 are specifically included: polyimide solution is made
Polyimide film, and it is carbonized 2 hours in 300 DEG C, 300 DEG C of argon atmospher are heated 2 hours, obtain carbon-fiber film, then by carbon fiber
It ties up film and immerses concentrated sulfuric acid ultrasound 1 hour, wash, it is dry, obtain 5-30 μm of carbon fiber；By Na2S2O3Solution and polyvinylpyrrolidine
Ketone mixing, is added concentrated hydrochloric acid, stirs 2 hours, and products therefrom filtering is washed with deionized, obtains Ryukyu.
Technical solution as a further improvement of that present invention, the step S2 are specifically included: the coloured glaze that will be prepared in step S1
It in the graphene oxide solution that ball is dispersed in, adds carbon fiber and is uniformly mixed, by mixed liquor under the conditions of -50 DEG C, freezing is dry
It is dry to obtain graphene oxide/carbon fiber/sulphur aeroge.
Technical solution as a further improvement of that present invention, the Ryukyu, the graphene and the carbon fiber quality
Than for Ryukyu: graphene: carbon fiber=10:50:1.
Technical solution as a further improvement of that present invention, the step S3 are specifically included: phosphoric acid is added in distilled water
Phosphoric acid solution is made, phosphoric acid solution is added in GO/CNF/S aeroge, is placed in water heating kettle and reacts 12 hours for 180 DEG C, filtering is washed
It washs, it is dry, obtain phosphorus doping graphene oxide carbon fiber/sulphur aeroge.
Technical solution as a further improvement of that present invention, the volume ratio of the phosphoric acid and the distilled water be 0.5:25~
3:25。
The present invention also provides the phosphorus doping graphene carbon fiber Ryukyu aeroges prepared by above-mentioned preparation method.
The present invention also provides above-mentioned phosphorus doping graphene carbon fiber Ryukyu aeroges as lithium sulfur battery anode material
Using.
Compared with prior art, beneficial effects of the present invention:
A kind of preparation method of phosphorus doping graphene carbon fiber Ryukyu aeroge of the invention, it is easy to operate, at low cost, suitable
In industrialized production；
Phosphorus doping graphene Ryukyu carbon fiber aerogel material of the invention, hole area is big, improves supporting for sulphur
Measure (15.8mg/cm2)；It can be the quick shuttle of lithium electronics as lithium sulfur battery anode material with three-dimensional porous structure
Channel is provided, charge-transfer resistance (PGCF/S:14.6 Ω, pure S:39.3 Ω) is greatly reduced；As lithium-sulphur cell positive electrode
Material has excellent chemical property, and specific capacity is up to 1156mAh/g (0.1C), good cycling stability (circulation 1000 times,
100%) coulombic efficiency reaches.
Phosphorus doping graphene Ryukyu carbon fiber aerogel material of the invention is as lithium sulfur battery anode material in application, sulphur
Loading it is high, be used for that cycle performance to be high when lithium-sulfur cell, energy density is high, the small positive electrode of resistance.
Detailed description of the invention
1 μm of SEM figure that Fig. 1 is the PGCF/S in the embodiment of the present invention 1；
5 μm of SEM figure that Fig. 2 is the PGCF/S in the embodiment of the present invention 1；
The EDS figure that Fig. 3 is the PGCF/S in the embodiment of the present invention 1；
Fig. 4 is the cyclic voltammetry curve that PGCF/S positive electrode is applied to lithium-sulfur cell in the embodiment of the present invention 2；
Fig. 5 is three times charging and discharging curve of PGCF/S positive electrode under the conditions of 0.1C in the embodiment of the present invention 2；
Fig. 6 be the embodiment of the present invention 2 in PGCF/S positive electrode 0.5C 1000 cycle performance figures；
It is the impedance curve of PGCF/S positive electrode and bright sulfur as anode that Fig. 7, which is in the embodiment of the present invention 2,.
Specific embodiment:
Following embodiment further illustrates the contents of the present invention, but should not be construed as limiting the invention.Without departing substantially from
In the case where spirit of that invention and essence, to modifications or substitutions made by the method for the present invention, step or condition, the present invention is belonged to
Range.Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.
Embodiment 1
A kind of preparation method of phosphorus doping graphene carbon fiber Ryukyu aeroge comprising following steps:
1) polyimide solution is made by polyimide film by electrostatic spinning technique, and it is small in 300 DEG C of carbonizations 2
When, 300 DEG C of argon atmospher are heated 2 hours, and carbon-fiber film is obtained.Carbon-fiber film is immersed into concentrated sulfuric acid ultrasound 1 hour, is washed, it is dry,
Obtain 5~30 μm of carbon fibers (CNF)；
2) by 100mL, 9.64mg/mL Na2S2O3Solution and 100mL polyvinylpyrrolidone (PVP, molecular weight :~
55000) it mixes, 0.8mL concentrated hydrochloric acid is added into mixed liquor, stir 2 hours.Products therefrom filtering, is washed with deionized, obtains
To Ryukyu；
3) Ryukyu 900mg is dispersed in the graphene oxide solution of 200mL 1mg/mL, then be added into mixed liquor
100mg carbon fiber is uniformly mixed.By mixed liquor under the conditions of -50 DEG C, freeze-drying obtains graphene oxide/carbon fiber/sulphur gas
Gel (GO/CNF/S)；
4) 0.68mg phosphoric acid is added in 25mL distilled water, phosphoric acid solution is added in 100mg aeroge, is placed in water heating kettle
180 DEG C are reacted 12 hours, and filtering washs drying, obtains phosphorus doping graphene oxide/carbon fiber/sulphur aeroge (PGO/CNF/
S)。
5) PGO/CNF/S aeroge is placed in water heating kettle, hydrazine hydrate reduction under the conditions of 90 DEG C obtains phosphorus doping graphene
Carbon fiber/sulphur aeroge (PGCF/S).
PGCF/S obtained is subjected to electron-microscope scanning and elemental analysis, as a result as shown in Figure 1-3, wherein, Fig. 1 PGCF/S
1 μm of SEM figure, it can be seen that the reticular structure of graphene is wrapped in Ryukyu；5 μm of SEM that Fig. 2 is PGCF/S scheme, it can be seen that
It is connected between graphene by carbon fiber, and aeroge has duct abundant；The EDS that Fig. 3 is PGCF/S schemes, in C, S, P, O tetra-
The content of element is as shown in right side pie chart in figure.
Embodiment 2
Battery assembly and test: phosphorus doping graphene Ryukyu carbon fiber aeroge is struck out into the electrode slice that diameter is 12mm
As anode, using metal lithium sheet as cathode, electrolyte is 1M LiTFSI/DOL:DME (1:1), the group in argon gas glove box
Dress up CR2032 button cell.At room temperature with scanning speed to carry out cyclic voltammetry (Fig. 4) under conditions of 0.1mV/s,
Charge-discharge test (Fig. 5) is carried out with the current density of 0.1C at room temperature, test result is shown, specific capacity 1156mAh/g.With
The current density of 1C carries out long circulating test (Fig. 6), and test result shows phosphorus doping graphene/Ryukyu/carbon fiber aeroge
(PGCF/S) it is used as anode, lithium-sulfur cell recycles 1000 times, and coulombic efficiency reaches 100%, with simple sulphur as battery
Anode is improved compared to cyclical stability.
Claims (8)
1. a kind of preparation method of phosphorus doping graphene carbon fiber Ryukyu aeroge, which is characterized in that itself the following steps are included:
S1: being made polyimide film for polyimide solution, and carbonization is heated in protective atmosphere, obtains carbon-fiber film, then by carbon fiber
Film immerses the concentrated sulfuric acid, and ultrasound is washed, dry, obtains carbon fiber；
By Na2S2O3Solution is mixed with polyvinylpyrrolidone, and concentrated hydrochloric acid is added, and is stirred, filtering, and deionized water washing obtains coloured glaze
Ball；
S2: in the graphene oxide solution that the Ryukyu prepared in S1 is dispersed in, the carbon fiber prepared in S1 is added, mixing is equal
It is even, it is freeze-dried to obtain graphene oxide/carbon fiber/sulphur aeroge；
S3: phosphoric acid solution is added in graphene oxide/carbon fiber/sulphur aeroge, is placed in water heating kettle and reacts, is filtered, is washed, is done
It is dry, obtain phosphorus doping graphene oxide carbon fiber/sulphur aeroge；
S4: by phosphorus doping graphene oxide carbon fiber/sulphur ball aeroge hydrazine hydrate reduction, phosphorus doping graphene carbon fiber coloured glaze is obtained
Ball aeroge.
2. a kind of preparation method of phosphorus doping graphene carbon fiber Ryukyu aeroge according to claim 1, feature exist
In the step S1 is specifically included: polyimide film is made in polyimide solution, and it is carbonized 2 hours in 300 DEG C, argon
300 DEG C of atmosphere are heated 2 hours, are obtained carbon-fiber film, then carbon-fiber film is immersed concentrated sulfuric acid ultrasound 1 hour, are washed, dry, are obtained
To 5-30 μm of carbon fiber；
By Na2S2O3Solution is mixed with polyvinylpyrrolidone, be added concentrated hydrochloric acid, stir 2 hours, products therefrom filtering, spend from
Sub- water washing, obtains Ryukyu.
3. a kind of preparation method of phosphorus doping graphene carbon fiber Ryukyu aeroge according to claim 1, feature exist
In the step S2 is specifically included: in the graphene oxide solution that the Ryukyu prepared in step S1 is dispersed in, adding carbon fiber
Dimension is uniformly mixed, and by mixed liquor under the conditions of -50 DEG C, freeze-drying obtains graphene oxide/carbon fiber/sulphur aeroge.
4. a kind of preparation method of phosphorus doping graphene carbon fiber Ryukyu aeroge according to claim 3, feature exist
In the mass ratio of, the Ryukyu, the graphene and the carbon fiber be Ryukyu: graphene: carbon fiber=10:50:1.
5. a kind of preparation method of phosphorus doping graphene carbon fiber Ryukyu aeroge according to claim 1, feature exist
In the step S3 is specifically included: phosphoric acid being added in distilled water, phosphoric acid solution is made, phosphoric acid is added in GO/CNF/S aeroge
Solution is placed in water heating kettle and reacts 12 hours for 180 DEG C, filter, washs, dry, obtains phosphorus doping graphene oxide carbon fiber/sulphur
Aeroge.
6. a kind of preparation method of phosphorus doping graphene carbon fiber Ryukyu aeroge according to claim 5, feature exist
In the volume ratio of the phosphoric acid and the distilled water is 0.5:25~3:25.
7. prepared by a kind of preparation method of phosphorus doping graphene carbon fiber Ryukyu aeroge as described in any of the above-described claim
Phosphorus doping graphene carbon fiber Ryukyu aeroge.
8. application of the phosphorus doping graphene carbon fiber Ryukyu's aeroge as lithium sulfur battery anode material in claim 7.
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| CN201811305616 | 2018-11-05 | ||
| CN2018113056164 | 2018-11-05 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112952055A (en) * | 2021-01-15 | 2021-06-11 | 贵州民族大学 | Two-dimensional structure selenium telluride modified carbon fiber electrode material and preparation method thereof |
| CN113184829A (en) * | 2021-04-01 | 2021-07-30 | 东华大学 | Preparation method of low-volume-shrinkage carbon nanofiber aerogel |
| CN114574890A (en) * | 2022-03-19 | 2022-06-03 | 南昌大学 | Self-formed phosphorus-doped redox graphene aerogel catalyst and preparation method and application thereof |
| CN115959856A (en) * | 2023-02-20 | 2023-04-14 | 中国科学院长春应用化学研究所 | Carbon fiber @ GO aerogel, and preparation method and application thereof |
-
2019
- 2019-03-15 CN CN201910198511.1A patent/CN110112374A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112952055A (en) * | 2021-01-15 | 2021-06-11 | 贵州民族大学 | Two-dimensional structure selenium telluride modified carbon fiber electrode material and preparation method thereof |
| CN113184829A (en) * | 2021-04-01 | 2021-07-30 | 东华大学 | Preparation method of low-volume-shrinkage carbon nanofiber aerogel |
| CN113184829B (en) * | 2021-04-01 | 2022-12-23 | 东华大学 | Preparation method of low-volume-shrinkage carbon nanofiber aerogel |
| CN114574890A (en) * | 2022-03-19 | 2022-06-03 | 南昌大学 | Self-formed phosphorus-doped redox graphene aerogel catalyst and preparation method and application thereof |
| CN115959856A (en) * | 2023-02-20 | 2023-04-14 | 中国科学院长春应用化学研究所 | Carbon fiber @ GO aerogel, and preparation method and application thereof |
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