CN110400916A - A kind of carbon fibre composite preparation method of two selenizings molybdenum nanometer sheet modification - Google Patents
A kind of carbon fibre composite preparation method of two selenizings molybdenum nanometer sheet modification Download PDFInfo
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- CN110400916A CN110400916A CN201910466506.4A CN201910466506A CN110400916A CN 110400916 A CN110400916 A CN 110400916A CN 201910466506 A CN201910466506 A CN 201910466506A CN 110400916 A CN110400916 A CN 110400916A
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M4/362—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
- H01M4/58—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
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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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to Transition-metal dichalcogenide-carbon material technical field, specially a kind of carbon fibre composite and preparation method thereof of two selenizing molybdenum nanometer sheets modification.The preparation process of the carbon fibre composite of two selenizing molybdenum nanometer sheets modification of the invention includes: molybdenum base carbon nano-fiber to be prepared by electrostatic spinning and high temperature cabonization method, then grow selenizing molybdenum nanometer sheet by heat treatment technics.The advantages that this method has yield big, and density is high, and purity is high is handled without subsequent handling, economic and environment-friendly.The carbon fibre composite of the present invention two selenizings molybdenum nanometer sheet modification obtained, is a kind of ideal kalium ion battery negative electrode material.
Description
[technical field]
The invention belongs to Transition-metal dichalcogenide-carbon material technical fields, and in particular to a kind of selenizing molybdenum nanometer sheet
The carbon fibre composite of the carbon fibre composite preparation method of modification, the two selenizing molybdenum nanometer sheets modification is a kind of reason
The potassium ion negative electrode material thought.
[background technique]
Carbon nano-fiber has the characteristics that high conductivity, high-specific surface area, makes it in electrode material, adsorbent material, catalysis
Agent carrier etc. is used widely.Electrostatic spinning is a kind of special fiber fabrication process, and polymer solution or melt exist
Jet spinning is carried out in strong electrical field.Under electric field action, the drop at syringe needle can be become cone from spherical shape, and from conical tip
Extension obtains fiber filaments.Electrostatic spinning is simple with its manufacturing device, cost of spinning is cheap, the various, technique that can spin substance classes
The advantages that controllable, it has also become effectively prepare one of main path of nano-fiber material.
Two-dimensional layer metal selenide shows excellent performance in many fields, such as narrower band gap, line width and more
Good electron hole separation etc..Therefore, metal selenium compound, especially two-dimensional layer metal selenide are also becoming new and are grinding
Study carefully one of forward position, attracts the concern of numerous researchers.Two selenizing molybdenums, belong to hexagonal crystal system, have the piece similar to sandwich
Layer structure, with strong Covalent bonding together between Se and Mo atom in layer, between layers loosely by faint Van der Waals force
It is combined together.But the surface energy of two selenizing molybdenums of sheet is relatively high, under Van der Waals interaction power, can be stacked on one
It rises, is unfavorable for electron-transport, and the distance between piece and piece are small, two pure selenizing molybdenums can be to two selenium of sheet when being used as battery material
Changing molybdenum has percussion, destroys laminated structure, and then cause cycle performance of battery poor.
Due to compound with the huge property potentiality for improving material between material, two selenizing molybdenum composite materials are also to work as
The hot spot of preceding research.Traditional two selenizing molybdenums/carbon composite preparation method is mostly sol-gel method, hydro-thermal method, co-precipitation
Method etc..But the chemical reaction of these liquid phase methods is complicated, it is difficult to control, and need the processes such as complicated subsequent purification.Phase therewith
Have than, physical gas phase deposition technology at low cost, preparation process is simple, and technological parameter controllability is strong, it can be achieved that industrial mass
The features such as amount production.
Of the invention is pyrolyzed into molybdenum base carbon nano-fiber using pre-oxidation polyacrylonitrile/ammonium molybdate nanofiber at high temperature
The characteristics of, in vacuum tube furnace, selenium powder is directly evaporated with heat treatment technics as selenium source, in the effect of carrier gas and high temperature
Under, obtain a kind of carbon nano-fiber composite material of two selenizing molybdenum nanometer sheets modification.The composite construction that this method is prepared
Material yield is big, and density is high, and purity is high is handled without subsequent handling, and preparation method is economic and environment-friendly.
[summary of the invention]
One of the objects of the present invention is to provide a kind of preparations of the carbon fibre composite of two selenizing molybdenum nanometer sheets modification
Method.The composite density that this method is prepared is high, and purity is high is not necessarily to subsequent processing；And this method have equipment and
The advantages that simple process, product yield is high, low in cost, production process clean and environmental protection
The second object of the present invention is to propose a kind of carbon fibre composite of two selenizing molybdenum nanometer sheets modification, this multiple
When condensation material is used for battery material, that is, the wider atom lamellar spacing of two selenizing molybdenums, which is utilized, facilitates the insertion and abjection of ion,
Battery capacity is improved, the high electric conductivity of carbon nano-fiber and steady point property is also utilized, promotes the cyclical stability of battery.
A kind of preparation method of the carbon fibre composite of two selenizings molybdenum nanometer sheet modification provided by the invention, feature exist
In using the characteristics of polyacrylonitrile/ammonium molybdate nanofiber is pyrolyzed into molybdenum base carbon nano-fiber at high temperature is pre-oxidized, in vacuum
In tube furnace, selenium powder is directly evaporated using heat treatment technics as selenium source, under the action of carrier gas and high temperature, has obtained one kind two
The carbon nano-fiber composite material of selenizing molybdenum nanometer sheet modification.
A kind of preparation method of the carbon fibre composite of two selenizings molybdenum nanometer sheet modification provided by the invention, including it is following
Step and content:
(1) polyacrylonitrile powder is added in n,N-Dimethylformamide solvent, under conditions of heating water bath, is continued
Stirring obtains uniformly sticky polyacrylonitrile dispersion liquid；
(2) ammonium molybdate powder is added to the polyacrylonitrile dispersion liquid that step (1) obtains, it is lasting to stir, it obtains uniform
Electrostatic spinning solution；
(3) electrostatic spinning solution for obtaining step (2) carries out electrostatic spinning, obtains polyacrylonitrile/ammonium molybdate Nanowire
Tie up precursor；
(4) polyacrylonitrile/ammonium molybdate nanofiber precursor that step (3) obtains is pre-oxidized in air, is stablized
Polyacrylonitrile, polyacrylonitrile/ammonium molybdate nanofiber after being pre-oxidized；
(5) polyacrylonitrile/ammonium molybdate nanofiber that step (4) obtains is subjected to pyrocarbon under the protection of inert gas
Change, obtains molybdenum base carbon nano-fiber；
(6) the molybdenum base carbon nano-fiber that step (5) obtains is ground, and with a certain amount of selenium powder mixing after the side of being put into
In boat, and this Noah's ark is put into position among tube furnace；
(7) by heat treatment technics using selenium powder as selenium source, under the action of carrier gas, the modification of two selenizing molybdenum nanometer sheets is obtained
Carbon nano-fiber composite material.
In the present invention, in step (1), the fine mass fraction of polypropylene is 6%~10% in the fine dispersion liquid of polypropylene；
In the present invention, in step (2), the ammonium molybdate powder that addition quality is equivalent to polyacrylonitrile quality 25%~35% is arrived
In the fine dispersion liquid of polypropylene, electrostatic spinning solution is obtained；
In the present invention, described in step (3), electrostatic spinning process parameter are as follows: electrostatic 12~20Kv of field voltage, spinning speed
0.3~0.6mL/h, receiving distance is 12-18cm；
In the present invention, step (4) is described, pre-oxidizing conditions are as follows: temperature is 150~200 DEG C, and soaking time is 10~14h；
In the present invention, step (5) is described, high-temperature process condition are as follows: inert gas (including but not limited to argon gas, nitrogen, helium
Gas) protection, temperature is 500~700 DEG C, and the time is 1~3h.
In the present invention, step (6) is described, and the mass ratio of selenium powder and molybdenum base carbon nano-fiber is 1:2~3；
In the present invention, step (7) is described, heat treatment technics condition are as follows: under the mixed gas of argon gas and hydrogen (95%
Argon gas/nitrogen/helium, 5% hydrogen), 250~300 DEG C are warming up to the rate of 3~5 DEG C/min, keeps the temperature 2~3h, then with 3
~5 DEG C/min is warming up to 600~800 DEG C, and keeps the temperature 1~2h.
Using scanning electron microscope (SEM), X-ray diffractometer (XRD), electrochemical workstation is made to characterize the present invention
The pattern and performance of the carbon nano-fiber composite material of standby obtained two selenizing molybdenum nanometer sheets modification, result are as follows:
(1) XRD test result shows selenizing molybdenum in 2 θ=13.7 °, 31.4 °, 37.9 °, 47.5 ° and 55.9 ° of diffraction maximum
It corresponds respectively to (002) of two selenizing molybdenums, (100), (103), (105) and (110) crystal face.Referring to attached drawing 1；
(2) SEM tests the carbon nano-fiber composite wood that structure shows the modification of two selenizing molybdenum nanometer sheets prepared by the present invention
Material, selenizing molybdenum nanometer sheet are equably grown on carbon fiber, restrained effectively the reunion of selenizing molybdenum itself, improve composite material
Electric conductivity.Referring to attached drawing 2 and Fig. 3；The present invention has the advantages that
It is a kind of effective efficiently preparation method 1. preparation process is simple, low in cost；
2. experimental design is ingenious.
(1) first, by electrostatic spinning and high temperature cabonization technology, carbon nano-fiber is simply and effectively prepared, effectively
Ground inhibits two selenizing molybdenums itself ground to reunite.Carbon nano-fiber has excellent electric conductivity, so that electronics can be in electrochemical process
It transmits effective and rapidly, so that the excellent properties of selenizing molybdenum nanometer sheet are fully used.
(2) second, the compound of one-dimensional material and two-dimensional material is realized by simple heat treatment technics, so that the two
Advantage is given full play to, to construct novel composite material.
(3) carbon fibre composite of two selenizings molybdenum nanometer sheet modification prepared by the present invention, is that kalium ion battery etc. is novel
The ideal electrode material of the energy.
[Detailed description of the invention]
(1) Fig. 1 is the XRD of the carbon fibre composite of the two selenizing molybdenum nanometer sheets modification of the embodiment of the present invention 1,2 and 3
Figure.
(2) Fig. 2 is the SEM image of the carbon fibre composite of the two selenizing molybdenum nanometer sheets modification of the embodiment of the present invention 4.
(3) Fig. 3 is the SEM image of the carbon fibre composite of the two selenizing molybdenum nanometer sheets modification of the embodiment of the present invention 5.
[specific embodiment]
Below with reference to specific example, the present invention is further explained, it should be appreciated that these examples be merely to illustrate the present invention without
For limiting the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art can
To make various changes or modification to the present invention, such equivalent forms equally fall within model defined by the application the appended claims
It encloses.
Embodiment 1
The present embodiment the following steps are included:
(1) 0.375g polyacrylonitrile powder is added to 4.5gN, in dinethylformamide solvent, in the condition of water-bath
Under, it is lasting to stir, uniform sticky dispersion liquid is prepared.
(2) ammonium molybdate of 0.1g is added in the sticky dispersion liquid of polyacrylonitrile, it is lasting to stir, it is molten to obtain electrostatic spinning
Liquid.
(3) obtained electrostatic spinning solution is subjected to electrostatic spinning, adjusts technological parameter are as follows: electrostatic field voltage 15Kv,
Spinning speed is 0.3 mL/min, receives distance 12cm, polyacrylonitrile/ammonium molybdate nanofiber precursor is prepared.
(4) obtained polyacrylonitrile/ammonium molybdate nanofiber precursor is pre-oxidized in air atmosphere, pre-oxidation
Temperature is 170 DEG C, and heating rate is 1 DEG C/min, preoxidation time 12h, polyacrylonitrile/molybdic acid after pre-oxidation is prepared
Ammonium nanofiber.
(5) polyacrylonitrile after obtained pre-oxidation/ammonium molybdate nanofiber is subjected to pyrocarbon in high-purity argon gas
Change, high temperature cabonization temperature is 600 DEG C, and the high temperature cabonization time is 1h, and molybdenum base carbon nano-fiber is prepared.
(6) it by after molybdenum base carbon nano-fiber obtained after 0.1g high temperature cabonization grinding, is mixed, is put with 0.3g selenium powder
Enter in Noah's ark.This Noah's ark is put into position among tube furnace, under conditions of the mixed gas of argon gas and hydrogen, is just started with 2
DEG C/heating rate of min is raised to 280 DEG C, and keeps the temperature 3h, 700 DEG C of heat preservation 2h are raised to the heating rate of 3 DEG C/min later, most
Composite material obtained is MoSe eventually2/C-1.Fig. 1 is the XRD diagram of embodiment 1.
Embodiment 2
By in embodiment 1, under conditions of the mixed gas of argon gas and hydrogen, last heating is changed to be raised to 600 DEG C,
Yu Juntong embodiment 1, final composite material obtained is MoSe2/C-2.Fig. 1 is the XRD diagram of embodiment 2.
Embodiment 3
By in embodiment 1, under conditions of the mixed gas of argon gas and hydrogen, last heating is changed to be raised to 800 DEG C,
Yu Juntong embodiment 1, final composite material obtained is MoSe2/C-3.Fig. 1 is the XRD diagram of embodiment 3.
Embodiment 4
The present embodiment the following steps are included:
(1) 0.375g polyacrylonitrile powder is added to 4.5gN, in dinethylformamide solvent, in the condition of water-bath
Under, it is lasting to stir, uniform sticky dispersion liquid is prepared.
(2) ammonium molybdate of 0.1g is added in the sticky dispersion liquid of polyacrylonitrile, it is lasting to stir, it is molten to obtain electrostatic spinning
Liquid.
(3) obtained electrostatic spinning solution is subjected to electrostatic spinning, adjusts technological parameter are as follows: electrostatic field voltage 15Kv,
Spinning speed is 0.3 mL/min, receives distance 12cm, polyacrylonitrile/ammonium molybdate nanofiber precursor is prepared.
(4) obtained polyacrylonitrile/ammonium molybdate nanofiber precursor is pre-oxidized in air atmosphere, pre-oxidation
Temperature is 170 DEG C, and heating rate is 1 DEG C/min, preoxidation time 12h, polyacrylonitrile/molybdic acid after pre-oxidation is prepared
Ammonium nanofiber.
(5) polyacrylonitrile after obtained pre-oxidation/ammonium molybdate nanofiber is subjected to pyrocarbon in high-purity argon gas
Change, high temperature cabonization temperature is 500 DEG C, and the high temperature cabonization time is 1h, and molybdenum base carbon nano-fiber is prepared.
(6) it by after molybdenum base carbon nano-fiber obtained after 0.1g high temperature cabonization grinding, is mixed, is put with 0.3g selenium powder
Enter in Noah's ark.
(7) this Noah's ark is put into position among tube furnace, under conditions of the mixed gas of argon gas and hydrogen, just started with
The heating rate of 2 DEG C/min is raised to 280 DEG C, and keeps the temperature 3h, is raised to 700 DEG C of heat preservation 2h later with the heating rate of 3 DEG C/min, most
Composite material obtained is MoSe eventually2/C-4.Fig. 2 is the SEM characterization image of embodiment 4.
Embodiment 5
By in embodiment 4, in the case where argon gas is the protective condition of inert gas, the temperature of carbonization is changed to 700 DEG C, remaining is same
Embodiment 4, final composite material obtained is MoSe2/C-5.Fig. 3 is the SEM characterization image of embodiment 5.
According to anode coat, potassium block, diaphragm, electrolyte, cathode, the sequence assembled battery of positive shell, in glove box
Kalium ion battery assembling is carried out, then in NEWARE test macro, in 100mA g-1Under current density, battery performance is tested.
As a result as shown in the table:
Claims (10)
1. a kind of carbon fibre composite preparation method of two selenizing molybdenum nanometer sheets modification, it is characterised in that: pass through electrostatic spinning
Polyacrylonitrile/ammonium molybdate nanofiber precursor is prepared, obtains molybdenum base carbon nano-fiber using preannealing and high temperature cabonization,
Two selenizing molybdenum nanometer sheets are grown on nanofiber finally by heat treatment technics；Specific step is as follows:
(1) polyacrylonitrile powder is added in n,N-Dimethylformamide solvent, under conditions of heating water bath, is persistently stirred
It mixes, obtains uniformly sticky polyacrylonitrile dispersion liquid；
(2) ammonium molybdate powder is added to the polyacrylonitrile dispersion liquid that step (1) obtains, it is lasting to stir, obtain uniform electrostatic
Spinning solution；
(3) electrostatic spinning solution for obtaining step (2) carries out electrostatic spinning, before obtaining polyacrylonitrile/ammonium molybdate nanofiber
Body；
(4) polyacrylonitrile/ammonium molybdate nanofiber precursor that step (3) obtains is pre-oxidized in air, stablizes poly- third
Alkene eyeball, polyacrylonitrile/ammonium molybdate nanofiber after being pre-oxidized；
(5) polyacrylonitrile/ammonium molybdate nanofiber that step (4) obtains is subjected to high temperature cabonization under the protection of inert gas,
Obtain molybdenum base carbon nano-fiber；
(6) the molybdenum base carbon nano-fiber that step (5) obtains is ground, and is put into Noah's ark after mixing with a certain amount of selenium powder
In, and this Noah's ark is put into position among tube furnace；
(7) by heat treatment, using selenium powder as selenium source, under the action of gaseous mixture (including hydrogen and inert gas), two are obtained
The carbon nano-fiber composite material of selenizing molybdenum nanometer sheet modification.
2. a kind of carbon fibre composite preparation method of two selenizings molybdenum nanometer sheet modification according to claim 1, special
Sign is in step (1) that the mass fraction of polyacrylonitrile is 6%~10% in polyacrylonitrile dispersion liquid.
3. a kind of carbon fibre composite preparation method of two selenizings molybdenum nanometer sheet modification according to claim 1, special
Sign is in step (2) that the quality of ammonium molybdate is equivalent to the 25%~35% of polyacrylonitrile quality.
4. a kind of carbon fibre composite preparation method of two selenizings molybdenum nanometer sheet modification according to claim 1, special
It levies and is in step (3), the electrostatic spinning process parameter are as follows: electrostatic 12~20kV of field voltage, the delivery rate of spinning solution
For 0.3~0.6mL/h, the distance of collecting board to needle point is 12-18cm.
5. a kind of carbon fibre composite preparation method of two selenizings molybdenum nanometer sheet modification according to claim 1, special
It levies and is in step (4), pre-oxidizing conditions are as follows: temperature is 150~200 DEG C, and soaking time is 10~14h.
6. a kind of carbon fibre composite preparation method of two selenizings molybdenum nanometer sheet modification according to claim 1, special
Sign is step (5) the high-temperature process condition are as follows: inert gas (including but not limited to argon gas, nitrogen, helium) protection, temperature
It is 500~700 DEG C, the time is 1~3h.
7. a kind of carbon fibre composite preparation method of two selenizings molybdenum nanometer sheet modification according to claim 1, special
Sign is that step (6) is described, and the mass ratio of selenium powder and molybdenum base carbon nano-fiber is 1:2~3.
8. a kind of carbon fibre composite preparation method of two selenizings molybdenum nanometer sheet modification according to claim 1, special
Sign is that step (7) is described, heat treatment condition are as follows: under the mixed gas of argon gas and hydrogen (95% argon gas/nitrogen/helium,
5% hydrogen), 250~300 DEG C are warming up to the rate of 3~5 DEG C/min, keeps the temperature 2~3h, then be warming up to 3~5 DEG C/min
600~800 DEG C, and keep the temperature 1~2h.
9. the carbon fiber composite that a kind of preparation method as described in one of claim 1-8 obtains the modification of two selenizing molybdenum nanometer sheets
Material.
10. as two selenizings molybdenum nanometer sheet as claimed in claim 9 modify carbon fibre composite can be used as high-performance potassium from
Sub- battery material.
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| CN116119626A (en) * | 2022-11-22 | 2023-05-16 | 湖南大学 | Synthesis method of C@MoSe2@NCNT material based on N-doped CNT structure |
| CN116314771A (en) * | 2023-05-12 | 2023-06-23 | 湖南镓睿科技有限公司 | High-surface-capacity potassium ion battery anode material and preparation method thereof |
| CN116314771B (en) * | 2023-05-12 | 2023-10-31 | 湖南镓睿科技有限公司 | High-surface-capacity potassium ion battery anode material and preparation method thereof |
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Application publication date: 20191101 |