CN105463831A - Molybdenum disulfide/graphene/carbon nanofiber composite material and preparation method thereof - Google Patents
Molybdenum disulfide/graphene/carbon nanofiber composite material and preparation method thereof Download PDFInfo
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- CN105463831A CN105463831A CN201510947452.5A CN201510947452A CN105463831A CN 105463831 A CN105463831 A CN 105463831A CN 201510947452 A CN201510947452 A CN 201510947452A CN 105463831 A CN105463831 A CN 105463831A
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M11/51—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
- 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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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The invention belongs to the technical field of transition metal sulfide-carbon materials and particularly provides a molybdenum disulfide/graphene/carbon nanofiber composite material and a preparation method thereof. The preparation method includes the steps that a polyacrylonitrile nanofiber membrane is prepared through electrostatic spinning, polyacrylonitrile nanofibers are wrapped with graphene oxide through a solution immersion method, then a graphene/carbon nanofiber composite membrane is prepared through high-temperature carbonization, and finally molybdenum disulfide nanosheets are grown on the graphene/carbon nanofibers in an in-situ mode through a one-step hydrothermal method. The molybdenum disulfide/graphene/carbon nanofiber composite material prepared through the method is controllable in morphology, has a high specific surface area and excellent electrical conductivity and can serve as an ideal high-performance electric catalytic material and an electrode material of a new-energy device such as a lithium ion battery and a solar cell.
Description
Technical field
The invention belongs to transient metal sulfide-material with carbon element technical field, be specifically related to a kind of molybdenum bisuphide/graphene/carbon nano-fiber composite material and preparation method thereof.
Background technology
Graphene is a kind of two-dimensional material only having an atomic thickness be made up of carbon atom, has very excellent physical and chemical performance, as higher inside carrier mobility (200000cm
2v
-1s
-1), good thermal conductivity (~ 5000Wm
-1k
-1), high transmission rate (~ 97.7%) and theoretical specific surface area (2630m
2g
-1), and the mechanical strength of excellence, be considered to one of potential nano material of current most.As a kind of one-dimensional carbon nano material, carbon nano-fiber has the advantages such as good mechanical property, larger specific area and good chemical stability, and these special natures make it be widely used in the fields such as the flexible base material of catalyst carrier, high molecule nano composite material, power conversion and memory device.Electrostatic spinning is a kind of technology simply and effectively preparing carbon nano-fiber, by high-pressure electrostatic, polymer solution is carried out spinning, then carry out pre-oxidation and high temperature cabonization can prepare the Static Spinning carbon nanofiber membrane with three-dimensional porous structure and high-specific surface area.The Graphene of high conductivity is wrapped in the electric conductivity that the carbon nano-fiber compared with bigger serface can improve further tunica fibrosa, is conducive to the transmission of electronics.
Molybdenum bisuphide is the Transition-metal dichalcogenide of a quasi-representative, and it belongs to hexagonal crystal system, and be very strong Mo-S covalent bond in layer, interlayer is more weak Van der Waals force.Molybdenum bisuphide has nontoxic, environmental friendliness, is easy to the advantages such as preparation, is paid close attention to widely and apply in the field such as catalytic hydrogen evolution and lithium ion battery electrode material.But pure molybdenum bisuphide is easy to reunite, and makes its avtive spot fully be exposed, has had a strong impact on the cyclical stability of its catalysis characteristics and stored energy.Therefore, the carbon nanomaterial of molybdenum bisuphide and excellent in stability is carried out effective compound significant.
The present invention, by simple technological design, prepares a kind of novel molybdenum bisuphide/graphene/carbon nano-fiber composite material.This composite has following advantage: Static Spinning carbon nano-fiber has unique three-dimensional porous structure, higher specific area and excellent mechanical property; Graphene parcel carbon nano-fiber can improve the electric conductivity of spinning film entirety, promotes the fast transport of electronics; Molybdenum disulfide nano sheet grows equably on graphene/carbon nanofiber, effectively can suppress the reunion of molybdenum bisuphide self, and its active edge is exposed more fully; The mechanical property of carbon nano-fiber excellence makes composite be applied in catalysis and energy storage device as flexible electrode material; Molybdenum bisuphide itself possesses higher catalytic activity and theoretical stored energy capacitance value, can improve catalytic performance and the stored energy performance of composites.Therefore, graphene/carbon nanofiber and molybdenum disulfide nano sheet are carried out effective compound, synergy good between three can be realized, to prepare the composite of excellent performance.
Summary of the invention
Molybdenum bisuphide/graphene/carbon nano-fiber composite material that the object of the present invention is to provide a kind of electrochemical performance and preparation method thereof.
Molybdenum bisuphide provided by the present invention/graphene/carbon nano-fiber composite material, its raw materials composition comprises: polyacrylonitrile,
n, N-dimethyl formamide, graphene oxide, molybdenum salt, sulfosalt etc.
Molybdenum bisuphide provided by the present invention/graphene/carbon nano-fiber composite material, its preparation process comprises: prepare polyacrylonitrile nanofiber film by electrostatic spinning, on polyacrylonitrile nanofiber, graphene oxide is wrapped up through solution infusion method, graphene/carbon nano-fiber composite film is prepared again, finally by one step hydro thermal method growth in situ molybdenum disulfide nano sheet on graphene/carbon nanofiber by high temperature cabonization.Concrete steps are as follows:
(1) polyacrylonitrile powder is joined
n, N-in solvent dimethylformamide, Keep agitation, obtains polyacrylonitrile dispersion liquid that is homogeneous, thickness;
(2) the polyacrylonitrile dispersion liquid obtained is carried out electrostatic spinning, obtain polyacrylonitrile nanofiber film;
(3) the polyacrylonitrile nanofiber film pre-oxidation in air atmosphere will obtained, obtains the polyacrylonitrile nanofiber film after pre-oxidation;
(4) the polyacrylonitrile nanofiber film after gained pre-oxidation is soaked in graphene oxide solution, obtain polyacrylonitrile nanofiber/graphene oxide composite membrane;
(5) gained polyacrylonitrile nanofiber/graphene composite film is carried out high temperature cabonization under inert gas shielding, obtain graphene/carbon nano-fiber composite film;
(6) molybdenum salt and sulfosalt are dissolved in solvent, prepare homogeneous salting liquid;
(7) salting liquid step (6) obtained and graphene/carbon nano-fiber composite film, by solvent thermal reaction, obtain molybdenum bisuphide/graphene/carbon nano-fiber composite material.
In the present invention, in the electrostatic spinning process described in step (2), technological parameter is: electrostatic field voltage 15 ~ 25kV, spinning speed 0.2 ~ 0.4mmmin
-1, receiving range 15 ~ 25cm.
In the present invention, in the 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, and preoxidation time is 1 ~ 2h.
In the present invention, in the solution immersion process described in step (4), the concentration of graphene oxide solution is 0.5 ~ 2mgmL
-1, soak time is 12 ~ 36h.
In the present invention, in the high temperature cabonization process described in step (5), described inert gas is high-purity argon gas or high pure nitrogen, and high temperature cabonization temperature is 800 ~ 1500 DEG C, and the high temperature cabonization time is 1 ~ 3h.
In the present invention, the salting liquid preparation process described in step (6), molybdenum salt comprises Ammonium Molybdate Tetrahydrate, ammonium thiomolybdate; Sulfosalt comprises thiocarbamide, ammonium thiomolybdate; The mass range of molybdenum salt is 3 ~ 30mgmL
-1; The mass range of sulfosalt is 3 ~ 50mgmL
-1, solvent be water or
n, N-dimethyl formamide.
In the present invention, the solvent thermal reaction described in step (7), reaction temperature is 180 ~ 240 DEG C, and the reaction time is 10 ~ 24h.
Use scanning electronic microscope (SEM), X-ray diffractometer (XRD), electrochemical workstation to characterize the structure and morphology of molybdenum bisuphide/graphene/carbon nano-fiber composite material that the present invention obtains, its result is as follows:
(1) SEM test result shows: in graphene/carbon nano-fiber composite film, and graphene sheet layer is closely wrapped in carbon nano-fiber on the surface.In molybdenum bisuphide/graphene/carbon nano-fiber composite material, molybdenum disulfide nano sheet grows equably on the graphene/carbon nanofiber of high-ratio surface sum high conductivity, effectively inhibit the reunion of molybdenum bisuphide self, its electro-chemical activity edge is fully exposed.See accompanying drawing 1;
(2) XRD test result shows, prepared graphene/carbon nano-fiber composite film has a wider diffraction maximum at ° place, 2 θ=26, corresponding to (002) crystal face of carbon nano-fiber and Graphene.Prepared molybdenum bisuphide/graphene/carbon nano-fiber composite material demonstrates the characteristic peak of molybdenum bisuphide, and in 2 θ=14 °, 32 °, 57 ° all have stronger diffraction maximum, corresponding to (002) (100) and (110) crystal face of molybdenum bisuphide.See accompanying drawing 2;
(3) electro-chemical test shows, prepared molybdenum bisuphide/graphene/carbon nano-fiber composite material has excellent electrochemical catalysis Hydrogen Evolution Performance, its initial overpotential is-0.09V, Tafel slope is 48.8mV/decade, is far superior to the performance of pure molybdenum bisuphide.See accompanying drawing 3.
The invention has the advantages that:
(1) preparation process is simple, is easy to operation, is a kind of convenient effective preparation method;
(2) substrate selected is the carbon nano-fiber composite membrane of Graphene parcel.The parcel of Graphene makes carbon nano-fiber have higher electric conductivity, is more conducive to the transmission of electronics.Graphene/carbon nanofiber has high specific area, and more site can be provided for molybdenum disulfide nano sheet growth;
(3) molybdenum bisuphide prepared by/graphene/carbon nano-fiber composite material has good pliability.Graphene, carbon nano-fiber and molybdenum disulfide nano sheet are carried out effective compound, the advantage of three can be made to be given full play to, thus successfully construct the composite with multilevel hierarchy.
Molybdenum bisuphide prepared by the present invention/graphene/carbon nano-fiber composite material, can be used as the ideal electrode material of high performance catalyst material and the new energy devices such as lithium ion battery, solar cell.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the molybdenum bisuphide/graphene/carbon nanofiber of embodiment 1 in the present invention: (A) graphene/carbon nano-fiber composite material; (B) molybdenum bisuphide/graphene/carbon nano-fiber composite material.
Fig. 2 is the XRD figure of the molybdenum bisuphide/graphene/carbon nano-fiber composite material of embodiment 1 in the present invention.
Fig. 3 is the molybdenum bisuphide/graphene/carbon nano-fiber composite material of the embodiment of the present invention 1 and the electrochemical catalysis Hydrogen Evolution Performance figure of molybdenum bisuphide, (A) linear sweep voltammetry curve (LSV), (B) Tafel curve.
Detailed description of the invention
Below in conjunction with instantiation, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition, after the content of having read the present invention's instruction, those skilled in the art can make various change or amendment to the present invention, and these equivalent form of values fall within the application's appended claims limited range equally.
embodiment 1,the present embodiment comprises the following steps:
(1) 1g polyacrylonitrile powder is joined 10mL
n, N-in solvent dimethylformamide, Keep agitation, prepares homogeneous thickness dispersion liquid.
(2) the polyacrylonitrile dispersion liquid obtained is carried out electrostatic spinning, its adjusting process parameter is: electrostatic field voltage 20kV, spinning speed 0.3mmmin
-1, receiving range 20cm, prepares polyacrylonitrile nanofiber film.
(3) the polyacrylonitrile spinning film obtained is carried out pre-oxidation in air atmosphere, the temperature of pre-oxidation is 250 DEG C, and heating rate is 1 DEG C of min
-1, preoxidation time is 1h, prepares the polyacrylonitrile nanofiber film after pre-oxidation.
(4) by the polyacrylonitrile nanofiber film after gained pre-oxidation at 1mgmL
-1soak 12h in graphene oxide solution, prepare polyacrylonitrile nanofiber/graphene oxide composite membrane.
(5) gained polyacrylonitrile nanofiber/graphene oxide composite membrane is carried out high temperature cabonization in high pure nitrogen, high temperature cabonization temperature is 800 DEG C, and the high temperature cabonization time is 2h, prepares graphene/carbon nano-fiber composite film.
(6) 90mg tetra-hydrated sulfuric acid ammonium and 166mg thiocarbamide are dissolved in 20mL deionized water, ultrasonic 5min, prepare homogeneous salting liquid.
(7) by the salting liquid for preparing and 1 × 1cm
2graphene/carbon nano-fiber composite film put into water heating kettle, in 200 DEG C, react 12h, after Temperature fall, take out tunica fibrosa and repeatedly clean repeatedly and drying with deionized water and ethanol, prepare molybdenum bisuphide/graphene/carbon nano-fiber composite material, be designated as GCNFMoS
2-1.
embodiment 2,change the molybdenum salt in embodiment 1 and sulfosalt into 10mg ammonium thiomolybdate, solvent changes 10mL into
n, N-dimethyl formamide, all the other are all with embodiment 1, and final obtained composite is designated as GCNFMoS
2-2.
embodiment 3,to change the molybdenum salt in embodiment 1 and sulfosalt into 20mg ammonium thiomolybdate in embodiment 1, solvent changes 10mL into
n, N-dimethyl formamide, all the other are all with embodiment 1, and final obtained composite is designated as GCNFMoS
2-3.
embodiment 4,to change the temperature of hydro-thermal reaction in embodiment 1 into 180 DEG C in embodiment 1, all the other are all with embodiment 1, and final obtained composite is designated as GCNFMoS
2-4.
In electro-chemical test, adopt three electrode test systems, the glass-carbon electrode modified with prepared hybrid material is for working electrode, and saturated calomel electrode is reference electrode, and graphite rod is to electrode, and electrolyte is 0.5MH
2sO
4.Before testing, in advance electrolyte is led to nitrogen 30min.Linear sweep voltammetry is adopted to study the electrocatalytic hydrogen evolution reactivity of hybrid material prepared in the present invention.
Claims (8)
1. the preparation method of molybdenum bisuphide/graphene/carbon nano-fiber composite material, it is characterized in that: prepare polyacrylonitrile nanofiber film by electrostatic spinning, on polyacrylonitrile nanofiber, graphene oxide is wrapped up through solution infusion method, graphene/carbon nano-fiber composite film is prepared again, finally by one step hydro thermal method growth in situ molybdenum disulfide nano sheet on graphene/carbon nanofiber by high temperature cabonization; Concrete steps are as follows:
(1) polyacrylonitrile powder is joined
n, N-in solvent dimethylformamide, Keep agitation, obtains polyacrylonitrile dispersion liquid that is homogeneous, thickness;
(2) the polyacrylonitrile dispersion liquid obtained is carried out electrostatic spinning, obtain polyacrylonitrile nanofiber film;
(3) by the pre-oxidation in air atmosphere of polyacrylonitrile spinning film, the polyacrylonitrile nanofiber film after pre-oxidation is obtained;
(4) the polyacrylonitrile nanofiber film after gained pre-oxidation is soaked in graphene oxide solution, obtain polyacrylonitrile nanofiber/graphene oxide composite membrane;
(5) gained polyacrylonitrile nanofiber/graphene composite film is carried out high temperature cabonization under inert gas shielding, obtain graphene/carbon nano-fiber composite film;
(6) molybdenum salt and sulfosalt are dissolved in solvent, prepare homogeneous salting liquid;
(7) salting liquid step (6) obtained and graphene/carbon nano-fiber composite film carry out solvent thermal reaction, and reaction temperature is 180 ~ 240 DEG C, and the reaction time is 10 ~ 24h; Obtain molybdenum bisuphide/graphene/carbon nano-fiber composite material.
2. the preparation method of molybdenum bisuphide according to claim 1/graphene/carbon nano-fiber composite material, it is characterized in that the electrostatic spinning described in step (2), its technological parameter is: electrostatic field voltage 15 ~ 25kV, spinning speed 0.2 ~ 0.4mmmin
-1, receiving range 15 ~ 25cm.
3. the preparation method of molybdenum bisuphide according to claim 1/graphene/carbon nano-fiber composite material, is characterized in that in the preoxidation process described in step (3), and heating rate is 1 ~ 2 DEG C of min
-1, the temperature of pre-oxidation is 250 ~ 300 DEG C, and preoxidation time is 1 ~ 2h.
4. the preparation method of molybdenum bisuphide according to claim 1/graphene/carbon nano-fiber composite material, is characterized in that the concentration of the graphene oxide solution described in step (4) is 0.5 ~ 2mgmL
-1, soak time is 12 ~ 36h.
5. the preparation method of molybdenum bisuphide according to claim 1/graphene/carbon nano-fiber composite material, it is characterized in that in the high temperature cabonization process described in step (5), described inert gas is high-purity argon gas or high pure nitrogen, high temperature cabonization temperature is 800 ~ 1500 DEG C, and the high temperature cabonization time is 1 ~ 3h.
6. the preparation method of molybdenum bisuphide according to claim 1/graphene/carbon nano-fiber composite material, is characterized in that, in step (6), described molybdenum salt comprises Ammonium Molybdate Tetrahydrate, ammonium thiomolybdate; Sulfosalt comprises thiocarbamide, ammonium thiomolybdate; The mass range of molybdenum salt is 3 ~ 30mgmL
-1; The mass range of sulfosalt is 3 ~ 50mgmL
-1; Solvent be water or
n, N-dimethyl formamide.
7. the molybdenum bisuphide prepared by the described preparation method of one of claim 1-6/graphene/carbon nano-fiber composite material.
8. molybdenum bisuphide/graphene/carbon nano-fiber composite material as claimed in claim 7 is as the application of high-performance electric catalysis material and the electrode material as lithium ion battery and solar cell.
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Cited By (12)
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|---|---|---|---|---|
| CN107681142A (en) * | 2017-09-29 | 2018-02-09 | 合肥工业大学 | A kind of molybdenum disulfide cladding carbon nano-fiber as lithium ion battery negative material and preparation method thereof |
| CN108288693A (en) * | 2017-12-22 | 2018-07-17 | 天津师范大学 | A kind of anode material of lithium-ion battery zinc-tin bimetallic sulfide and the preparation method and application thereof |
| CN108442114A (en) * | 2018-02-07 | 2018-08-24 | 东华大学 | A kind of poly-triphenylamine-carbon nano-fiber composite material and its preparation and application |
| CN108607594A (en) * | 2018-05-08 | 2018-10-02 | 河北北方学院 | A kind of coppe ferrite/carbon nano-fiber/nitrogen-doped graphene composite electro catalytic material |
| 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 |
| 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 |
| CN111129394A (en) * | 2019-12-02 | 2020-05-08 | 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 |
| WO2021036219A1 (en) * | 2019-08-28 | 2021-03-04 | 青岛大学 | Molybdenum disulfide/graphene/carbon composite material and use 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 |
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| CN113981673A (en) * | 2021-09-03 | 2022-01-28 | 兰州大学 | 1T growing on carbon fiberPhase MoS2Preparation method and application of @ rGO composite material |
| CN114507981A (en) * | 2022-01-28 | 2022-05-17 | 南京工业大学 | Preparation method of graphene/molybdenum disulfide composite fiber fabric |
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| 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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| CN108607594A (en) * | 2018-05-08 | 2018-10-02 | 河北北方学院 | A kind of coppe ferrite/carbon nano-fiber/nitrogen-doped graphene composite electro catalytic material |
| 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 |
| US20220243366A1 (en) * | 2019-08-28 | 2022-08-04 | Qingdao University | Molybdenum disulfide/graphene/carbon composite material and use thereof |
| WO2021036219A1 (en) * | 2019-08-28 | 2021-03-04 | 青岛大学 | Molybdenum disulfide/graphene/carbon composite material and use thereof |
| CN111129394A (en) * | 2019-12-02 | 2020-05-08 | 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 |
| 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 |
| CN113787887A (en) * | 2021-08-27 | 2021-12-14 | 西安理工大学 | Vehicle-mounted air purifier |
| CN113981673A (en) * | 2021-09-03 | 2022-01-28 | 兰州大学 | 1T growing on carbon fiberPhase MoS2Preparation method and application of @ rGO composite material |
| CN114507981A (en) * | 2022-01-28 | 2022-05-17 | 南京工业大学 | Preparation method of graphene/molybdenum disulfide composite fiber fabric |
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