CN105463831B - A kind of molybdenum disulfide/graphene/carbon nano-fiber composite material and preparation method thereof - Google Patents
A kind of molybdenum disulfide/graphene/carbon nano-fiber composite material and preparation method thereof Download PDFInfo
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- CN105463831B CN105463831B CN201510947452.5A CN201510947452A CN105463831B CN 105463831 B CN105463831 B CN 105463831B CN 201510947452 A CN201510947452 A CN 201510947452A CN 105463831 B CN105463831 B CN 105463831B
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
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- D06M11/53—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
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- D06M2101/40—Fibres of carbon
Abstract
The invention belongs to transient metal sulfide-carbon material technical field, specially a kind of molybdenum disulfide/graphene/carbon nano-fiber composite material and preparation method thereof.Preparation method of the present invention includes: that polyacrylonitrile nanofiber film is prepared by electrostatic spinning, graphene oxide is wrapped up on polyacrylonitrile nanofiber by solution infusion method, graphene/carbon nano-fiber composite film is prepared by high temperature cabonization again, finally by one step hydro thermal method on graphene/carbon nanofiber growth in situ molybdenum disulfide nano sheet.Molybdenum disulfide prepared by the present invention/graphene/carbon nano-fiber composite material morphology controllable, specific surface area with higher and excellent electric conductivity can be used as the electrode material of a kind of ideal high-performance electric catalysis material and the new energy devices such as lithium ion battery and solar battery.
Description
Technical field
The invention belongs to transient metal sulfide-carbon material technical fields, and in particular to and a kind of molybdenum disulfide/graphene/
Carbon nano-fiber composite material and preparation method thereof.
Background technique
Graphene is a kind of two-dimensional material of only one atomic thickness being made of carbon atom, has very excellent object
Physicochemical performance, such as higher internal carrier mobility (200000 cm2V-1s-1), good thermal conductivity (~ 5000 W m-1
K-1), high transparency (~ 97.7%) and theoretical specific surface area (2630 m2 g-1) and excellent mechanical strength, it is considered to be when
One of modern most potential nano material.As a kind of one-dimensional carbon nano material, carbon nano-fiber has good mechanical property
The advantages that energy, biggish specific surface area and good chemical stability, these special natures make it be widely used in catalyst load
Body, high molecule nano composite material, energy are converted and the fields such as the flexible base material of memory device.Electrostatic spinning is a kind of letter
Technology that is single and effectively preparing carbon nano-fiber, carries out spinning for polymer solution by high-pressure electrostatic, then carry out pre-oxidation and
The Static Spinning carbon nanofiber membrane with three-dimensional porous structure and high-specific surface area can be prepared in high temperature cabonization.By high conductivity
Graphene be wrapped in the electric conductivity that can be further improved tunica fibrosa on the carbon nano-fiber of large specific surface area, be conducive to electricity
The transmission of son.
Molybdenum disulfide is a kind of typical Transition-metal dichalcogenide, it belongs to hexagonal crystal system, is very strong Mo- in layer
S covalent bond, interlayer are weaker Van der Waals forces.Molybdenum disulfide has many advantages, such as nontoxic, environmental-friendly, easily prepared, is being catalyzed
It is widely paid close attention to and is applied in the fields such as liberation of hydrogen and lithium ion battery electrode material.But pure molybdenum disulfide is easy to reunite, and makes
Its active site is unable to get abundant exposure, has seriously affected the cyclical stability of its catalysis characteristics and energy stores.Therefore, will
The carbon nanomaterial of molybdenum disulfide and excellent in stability carries out effectively compound be of great significance.
A kind of novel molybdenum disulfide/graphene/carbon nanofiber is prepared by simple technological design in the present invention
Composite material.The composite material has the advantage that Static Spinning carbon nano-fiber has unique three-dimensional porous structure, higher
Specific surface area and excellent mechanical property；The electric conductivity of spinning film entirety can be improved in graphene package carbon nano-fiber, promotes electricity
The quick transmission of son；Molybdenum disulfide nano sheet is equably grown on graphene/carbon nanofiber, and molybdenum disulfide can be effectively suppressed
The reunion of itself exposes its active edge more fully；The excellent mechanical property of carbon nano-fiber makes composite material
It is applied in catalysis and energy storage device as flexible electrode material；Molybdenum disulfide itself has higher catalytic activity and reason
By stored energy capacitance value, the catalytic performance and energy stores performance of composite material entirety can be improved.Therefore, by graphene/carbon nanometer
Fiber and molybdenum disulfide nano sheet progress are effectively compound, good synergistic effect between three may be implemented, to prepare performance
Excellent composite material.
Summary of the invention
It is multiple that the purpose of the present invention is to provide a kind of molybdenum disulfide of electrochemical performance/graphene/carbon nanofibers
Condensation material and preparation method thereof.
Molybdenum disulfide provided by the present invention/graphene/carbon nano-fiber composite material, preparing raw material composition includes:
Polyacrylonitrile,N,N-Dimethylformamide, graphene oxide, molybdenum salt, sulfosalt etc..
Molybdenum disulfide provided by the present invention/graphene/carbon nano-fiber composite material, preparation process include: to pass through
Polyacrylonitrile nanofiber film is prepared in electrostatic spinning, wraps up oxidation on polyacrylonitrile nanofiber by solution infusion method
Graphene, then graphene/carbon nano-fiber composite film is prepared by high temperature cabonization, finally by one step hydro thermal method in graphite
Growth in situ molybdenum disulfide nano sheet on alkene/carbon nano-fiber.Specific step is as follows:
(1) polyacrylonitrile powder is added toN,N-It is lasting to stir in solvent dimethylformamide, it obtains uniform, sticky
Polyacrylonitrile dispersion liquid；
(2) obtained polyacrylonitrile dispersion liquid is subjected to electrostatic spinning, obtains polyacrylonitrile nanofiber film；
(3) obtained polyacrylonitrile nanofiber film is pre-oxidized in air atmosphere, the polypropylene after being pre-oxidized
Nitrile nanofibre film；
(4) the polyacrylonitrile nanofiber film after pre-oxidizing gained impregnates in graphene oxide solution, obtains poly- third
Alkene nitrile nanofibre/graphene oxide composite membrane；
(5) gained polyacrylonitrile nanofiber/graphene composite film is subjected to high temperature cabonization under inert gas protection, is obtained
To graphene/carbon nano-fiber composite film；
(6) molybdenum salt and sulfosalt are dissolved in solvent, uniform salting liquid is prepared；
(7) salting liquid for obtaining step (6) and graphene/carbon nano-fiber composite film are obtained by solvent thermal reaction
Molybdenum disulfide/graphene/carbon nano-fiber composite material.
In the present invention, during electrostatic spinning described in step (2), technological parameter are as follows: 15 ~ 25 kV of electrostatic field voltage is spun
0.2 ~ 0.4 mm min of silk speed-1, receive 15 ~ 25 cm of distance.
In the present invention, in preoxidation process described in step (3), heating rate is 1 ~ 2 DEG C of min-1, the temperature of pre-oxidation is
250 ~ 300 DEG C, preoxidation time is 1 ~ 2 h.
In the present invention, in solution soaking process described in step (4), the concentration of graphene oxide solution is 0.5 ~ 2mg
mL-1, soaking time is 12 ~ 36 h.
In the present invention, during high temperature cabonization described in step (5), the inert gas is high-purity argon gas or High Purity Nitrogen
Gas, high temperature cabonization temperature are 800 ~ 1500 DEG C, and the high temperature cabonization time is 1 ~ 3 h.
In the present invention, salting liquid preparation process described in step (6), molybdenum salt includes Ammonium Molybdate Tetrahydrate, ammonium thiomolybdate；
Sulfosalt includes thiocarbamide, ammonium thiomolybdate；The mass range of molybdenum salt is 3 ~ 30 mg mL-1；The mass range of sulfosalt is 3 ~ 50 mg
mL-1, solvent be water orN,N-Dimethylformamide.
In the present invention, solvent thermal reaction described in step (7), reaction temperature is 180 ~ 240 DEG C, and the reaction time is 10 ~ 24
h。
The present invention is characterized using scanning electron microscope (SEM), X-ray diffractometer (XRD), electrochemical workstation to be obtained
Molybdenum disulfide/graphene/carbon nano-fiber composite material the structure and morphology obtained, result are as follows:
(1) SEM test result shows: in graphene/carbon nano-fiber composite film, graphene sheet layer is tightly wrapped
On carbon nano-fiber surface.In molybdenum disulfide/graphene/carbon nano-fiber composite material, molybdenum disulfide nano sheet is equably
It is grown on the graphene/carbon nanofiber of high-specific surface area and high conductivity, effectively inhibits the reunion of molybdenum disulfide itself,
Expose its electro-chemical activity edge sufficiently.Referring to attached drawing 1；
(2) XRD test result show prepared graphene/carbon nano-fiber composite film have at 2 θ=26 ° one compared with
Wide diffraction maximum, (002) crystal face corresponding to carbon nano-fiber and graphene.Prepared molybdenum disulfide/graphene/carbon nanometer
Fibrous composite shows the characteristic peak of molybdenum disulfide, and in 2 θ=14 °, 32 °, 57 ° have stronger diffraction maximum, corresponds to
(002) (100) and (110) crystal face of molybdenum disulfide.Referring to attached drawing 2；
(3) it is excellent to show that prepared molybdenum disulfide/graphene/carbon nano-fiber composite material has for electro-chemical test
Electrochemical catalysis Hydrogen Evolution Performance, starting overpotential be -0.09 V, Tafel slope be 48.8 mV/decade, far superior to
The performance of pure molybdenum disulfide.Referring to attached drawing 3.
The present invention has the advantages that
(1) preparation process is simple, easily operated, is a kind of convenient effective preparation method；
(2) substrate selected is the carbon nano-fiber composite membrane of graphene package.The package of graphene is so that carbon Nanowire
Dimension has higher electric conductivity, is more advantageous to the transmitting of electronics.Graphene/carbon nanofiber has high specific surface area, can be with
More sites are provided to grow for molybdenum disulfide nano sheet；
(3) molybdenum disulfide/graphene/carbon nano-fiber composite material prepared by has preferable flexibility.By graphite
Alkene, carbon nano-fiber and molybdenum disulfide nano sheet progress are effectively compound, and the advantage of three can be enable to give full play to, thus success
The composite material with multilevel structure is constructed.
Molybdenum disulfide prepared by the present invention/graphene/carbon nano-fiber composite material, can be used as high performance catalyst material
And the ideal electrode material of the new energy devices such as lithium ion battery, solar battery.
Detailed description of the invention
Fig. 1 is molybdenum disulfide/graphene/carbon nanofiber SEM figure of embodiment 1 in the present invention: (A) graphene/carbon
Nano-fiber composite material；(B) molybdenum disulfide/graphene/carbon nano-fiber composite material.
Fig. 2 is molybdenum disulfide/graphene/carbon nano-fiber composite material XRD diagram of embodiment 1 in the present invention.
Fig. 3 is molybdenum disulfide/graphene/carbon nano-fiber composite material and molybdenum disulfide electricity of the embodiment of the present invention 1
Chemical catalysis Hydrogen Evolution Performance figure, (A) linear sweep voltammetry curve (LSV), (B) Tafel curve.
Specific embodiment
Below with reference to specific example, the present invention is further explained.It should be understood that these embodiments be merely to illustrate the present invention and
It is not used in and limits the scope of the invention.In addition, after reading the content taught by the present invention, those skilled in the art can be right
The present invention makes various changes or modification, and these equivalent forms also fall within the scope of the appended claims of the present application.
Embodiment 1, the present embodiment the following steps are included:
(1) 1 g polyacrylonitrile powder is added to 10 mLN,N-It is lasting to stir in solvent dimethylformamide, preparation
Obtain uniform sticky dispersion liquid.
(2) obtained polyacrylonitrile dispersion liquid is subjected to electrostatic spinning, adjusts technological parameter are as follows: electrostatic field voltage 20
KV, 0.3 mm min of spinning speed-1, 20 cm of distance is received, polyacrylonitrile nanofiber film is prepared.
(3) obtained polyacrylonitrile spinning film being pre-oxidized in air atmosphere, the temperature of pre-oxidation is 250 DEG C,
Heating rate is 1 DEG C of min-1, preoxidation time 1h, the polyacrylonitrile nanofiber film after pre-oxidation is prepared.
(4) the polyacrylonitrile nanofiber film after pre-oxidizing gained is in 1 mg mL-112 are impregnated in graphene oxide solution
Polyacrylonitrile nanofiber/graphene oxide composite membrane is prepared in h.
(5) gained polyacrylonitrile nanofiber/graphene oxide composite membrane is subjected to high temperature cabonization in high pure nitrogen, it is high
Warm carburizing temperature is 800 DEG C, and the high temperature cabonization time is 2 h, and graphene/carbon nano-fiber composite film is prepared.
(6) 90 mg, tetra- hydrated sulfuric acid ammonium and 166 mg thiocarbamides are dissolved in 20mL deionized water, 5 min of ultrasound are prepared into
To uniform salting liquid.
(7) by the salting liquid being prepared and 1 × 1 cm2Graphene/carbon nano-fiber composite film be put into water heating kettle,
12h is reacted in 200 DEG C, after Temperature fall, tunica fibrosa is taken out and cleans multiple and drying repeatedly with deionized water and ethyl alcohol,
Molybdenum disulfide/graphene/carbon nano-fiber composite material is prepared, is denoted as GCNF@MoS2-1。
Embodiment 2, by embodiment 1 molybdenum salt and sulfosalt change 10 mg ammonium thiomolybdates into, solvent changes 10 mL intoN,N-
Dimethylformamide, with embodiment 1, final composite material obtained is denoted as GCNF@MoS for remaining2-2。
Embodiment 3, by embodiment 1 by embodiment 1 molybdenum salt and sulfosalt change 20 mg ammonium thiomolybdates, solvent into
Change 10 mL intoN,N-Dimethylformamide, with embodiment 1, final composite material obtained is denoted as GCNF@MoS for remaining2-
3。
Embodiment 4 changes the temperature by hydro-thermal reaction in embodiment 1 in embodiment 1 into 180 DEG C, remaining is the same as implementation
Example 1, final composite material obtained are denoted as GCNF@MoS2-4。
In electro-chemical test, using three electrode test systems, it is with the glass-carbon electrode that prepared hybrid material is modified
Working electrode, saturated calomel electrode are reference electrode, and graphite rod is to electrode, and electrolyte is 0.5 M H2SO4.Before testing, in advance
Electrolyte is first led into 30 min of nitrogen.Using the electro-catalysis of hybrid material prepared in the linear sweep voltammetry research present invention
Evolving hydrogen reaction activity.
Claims (8)
1. a kind of molybdenum disulfide/graphene/carbon nano-fiber composite material preparation method, it is characterised in that: pass through Static Spinning
Polyacrylonitrile nanofiber film is prepared in silk, and graphite oxide is wrapped up on polyacrylonitrile nanofiber by solution infusion method
Alkene, then graphene/carbon nano-fiber composite film is prepared by high temperature cabonization, finally by one step hydro thermal method graphene/
Growth in situ molybdenum disulfide nano sheet on carbon nano-fiber composite membrane；Specific step is as follows:
(1) polyacrylonitrile powder is added toN,N-It is lasting to stir in solvent dimethylformamide, obtain uniform, sticky gather
Acrylonitrile dispersion liquid；
(2) obtained polyacrylonitrile dispersion liquid is subjected to electrostatic spinning, obtains polyacrylonitrile nanofiber film；
(3) polyacrylonitrile spinning film is pre-oxidized in air atmosphere, the polyacrylonitrile nanofiber film after being pre-oxidized；
(4) the polyacrylonitrile nanofiber film after pre-oxidizing gained impregnates in graphene oxide solution, obtains polyacrylonitrile
Nanofiber/graphene oxide composite membrane；
(5) gained polyacrylonitrile nanofiber/graphene composite film is subjected to high temperature cabonization under inert gas protection, obtains stone
Black alkene/carbon nano-fiber composite membrane；
(6) molybdenum salt and sulfosalt are dissolved in solvent, uniform salting liquid is prepared；
(7) salting liquid for obtaining step (6) and graphene/carbon nano-fiber composite film carry out hydro-thermal reaction, and reaction temperature is
180 ~ 240 DEG C, the reaction time is 10 ~ 24 h；Obtain molybdenum disulfide/graphene/carbon nano-fiber composite material.
2. molybdenum disulfide according to claim 1/graphene/carbon nano-fiber composite material preparation method, feature
It is electrostatic spinning described in step (2), technological parameter are as follows: 15 ~ 25 kV of electrostatic field voltage, 0.2 ~ 0.4 mm of spinning speed
min-1, receive 15 ~ 25 cm of distance.
3. molybdenum disulfide according to claim 1/graphene/carbon nano-fiber composite material preparation method, feature
It is in preoxidation process described in step (3), heating rate is 1 ~ 2 DEG C of min-1, the temperature of pre-oxidation is 250 ~ 300 DEG C, in advance
Oxidization time is 1 ~ 2 h.
4. molybdenum disulfide according to claim 1/graphene/carbon nano-fiber composite material preparation method, feature
The concentration for being graphene oxide solution described in step (4) is 0.5 ~ 2mg mL-1, soaking time is 12 ~ 36 h.
5. molybdenum disulfide according to claim 1/graphene/carbon nano-fiber composite material preparation method, feature
It is during high temperature cabonization described in step (5), the inert gas is high-purity argon gas or high pure nitrogen, high temperature cabonization temperature
It is 800 ~ 1500 DEG C, the high temperature cabonization time is 1 ~ 3 h.
6. molybdenum disulfide according to claim 1/graphene/carbon nano-fiber composite material preparation method, feature
It is in step (6), the molybdenum salt includes Ammonium Molybdate Tetrahydrate or ammonium thiomolybdate；Sulfosalt includes thiocarbamide or ammonium thiomolybdate；
The concentration range of molybdenum salt is 3 ~ 30 mg mL-1；The concentration range of sulfosalt is 3 ~ 50 mg mL-1；Solvent be water orN,N-Dimethyl
Formamide.
7. a kind of molybdenum disulfide that the preparation method as described in one of claim 1-6 is prepared/graphene/carbon nanofiber is answered
Condensation material.
8. molybdenum disulfide as claimed in claim 7/graphene/carbon nano-fiber composite material is as high-performance electric catalysis material
And the application as lithium ion battery and the electrode material of solar battery.
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| CN107681142B (en) * | 2017-09-29 | 2020-11-27 | 合肥工业大学 | Molybdenum disulfide coated carbon nanofiber used as lithium ion battery negative electrode material and preparation method thereof |
| CN108288693B (en) * | 2017-12-22 | 2020-07-10 | 天津师范大学 | Zinc-tin bimetallic sulfide as negative electrode material of sodium-ion battery and preparation method and application thereof |
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| CN108771981A (en) * | 2018-06-04 | 2018-11-09 | 郑州新世纪材料基因组工程研究院有限公司 | Graphene composite material and its preparation method and application, graphene-carbon nano-fiber film and preparation method thereof |
| CN108766782A (en) * | 2018-06-13 | 2018-11-06 | 常熟理工学院 | A kind of preparation method of fiber/graphene/molybdenum sulfide flexible electrode material |
| CN110504431B (en) * | 2019-08-28 | 2020-04-14 | 青岛大学 | Molybdenum disulfide/graphene/carbon composite material and application thereof |
| CN111129394B (en) * | 2019-12-02 | 2022-08-19 | 深圳石墨烯创新中心有限公司 | Functional composite type carbon nanofiber/graphene membrane as well as preparation method and application thereof |
| CN112473711A (en) * | 2020-11-20 | 2021-03-12 | 新疆大学 | Preparation method of molybdenum disulfide/nitrogen and phosphorus co-doped coal-based carbon fiber composite material |
| CN113787887B (en) * | 2021-08-27 | 2023-08-01 | 西安理工大学 | Vehicle-mounted air purifier |
| CN113981673B (en) * | 2021-09-03 | 2023-05-12 | 兰州大学 | Growth 1T on carbon fiberPhase MoS 2 Preparation method and application of composite material @ rGO |
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