CN105742074A - Poly-dopamine based porous carbon fiber/MoSe2 composite material and preparation method thereof - Google Patents
Poly-dopamine based porous carbon fiber/MoSe2 composite material and preparation method thereof Download PDFInfo
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- CN105742074A CN105742074A CN201610199883.2A CN201610199883A CN105742074A CN 105742074 A CN105742074 A CN 105742074A CN 201610199883 A CN201610199883 A CN 201610199883A CN 105742074 A CN105742074 A CN 105742074A
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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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
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- 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
The invention belongs to the technical field of a composite fiber material, in particular relates to a poly-dopamine based porous carbon fiber/MoSe2 nanosheet composite material and a preparation method thereof. The method comprises the following steps of preparing a spinning solution with a spinnable high-polymer material, and preparing to obtain porous fiber with an uniform structure by an electrostatic spinning device; immersing the porous fiber in a dopamine solution, and controlling the thickness of a poly-dopamine cladding layer by adjusting the concentration and the reaction time of the dopamine solution; carrying out high-temperature carbonization to achieve carbonization on the poly-dopamine modified porous fiber material; and uniformly arranging MoSe2 nanosheets on the surface of the porous fiber by a hydrothermal method. The method disclosed by the invention is safe and environment-friendly, and the prepared porous carbon fiber/MoSe2 has the advantages of high active substance content, high specific area, high conductivity, stable physical and chemical performance and the like, and is an ideal electrode material for preparing an active electric catalyst for a hydrogen evolution reaction.
Description
Technical field
The invention belongs to complex fiber material technical field, be specifically related to a kind of porous carbon fiber/bis-selenizing molybdenum composite material and preparation method thereof.
Background technology
Nanofiber is the Typical Representative of monodimension nanometer material, and electrostatic spinning technique is as a kind of method that directly can prepare polymer nanofiber continuously, all the time extensively concerned.The nano fibrous membrane prepared is because of advantages such as it has good stability, porosity is high, specific surface area is big, conductivity is high and more material and electric transmission ducts; can be widely applied to the electrode material etc. of catalyst carrier, hydrogen storage material, adsorbing material and ultracapacitor or lithium ion battery, advantageously account for energy crisis and the problem of environmental pollution of society.
Traditional electrostatic spinning nano fiber smooth surface, structure is single, is difficult to meet the demand of practical application.The introducing of loose structure, adds the specific surface area of fibrous material, is also conducive to improving the surface activity of material.The preparation method that present invention firstly provides the loose structure carbon fibre material based on poly-dopamine, it is intended to the deficiency of traditional fibre material can be made up by the preparation of this novel fibrous material with multistage pore space structure, to being applied in more areas.
Two selenizing molybdenum (MoSe2) for a kind of two-dimentional Transition-metal dichalcogenide with graphite-like structure.In its monolayer Se atom and Mo atom by three layers covalent bond form tightly packed become " Se-Mo-Se " sandwich type structural, interlayer is interacted by Van der Waals force.The interlayer structure of this kind graphite makes sudden and violent leakage Se atom outside and Mo atom have good chemism.The present invention prepares porous carbon fiber material in conjunction with the self-polymeric reaction of Static Spinning technology and poly-dopamine.Solvent-thermal method is utilized to grow MoSe at porous fibre surface in situ2Nanoscale twins, is successfully realized one-dimensional porous carbon fiber and two dimension MoSe2Controlled the constructing of nanoscale twins multilevel hierarchy composite.This composite has the advantage that the prepared loose structure carbon fiber based on poly-dopamine has bigger specific surface area, by it as MoSe2The matrix material of nanometer sheet growth, it is possible to effectively prevent MoSe2Nanometer sheet is reunited；Furthermore the loose structure carbon fiber based on poly-dopamine has excellent electric conductivity, be conducive to the quick transmission of ion and electronics, MoSe2There is excellent catalytic performance and higher capacity and energy density, the two is effectively constructed, it is possible to maximize favourable factors and minimize unfavourable ones, effectively given play to respective advantage.
Summary of the invention
It is an object of the invention to provide novel porous carbon fiber/bis-selenizing molybdenum composite material that a kind of preparation process is simple, preparation cost is cheap and preparation method thereof.
Porous carbon fiber/bis-selenizing molybdenum composite material provided by the present invention, it is prepared raw material composition and includes: can spin macromolecule, dopamine, selenium simple substance, molybdenum salt.
Porous carbon fiber/bis-selenizing molybdenum composite material provided by the present invention, selecting Static Spinning porous fibre is substrate, uploads two selenizing molybdenums by the oxidation self-polymeric reaction of dopamine and the last hydro-thermal of high temperature cabonization process and prepares.
The present invention is to provide a kind of high-specific surface area, high porosity, the carbon fiber loaded two selenizing molybdenum composite materials of loose structure that obtained by poly-dopamine shell carbonization.
Porous carbon fiber/bis-selenizing molybdenum composite material provided by the present invention, its preparation process includes: obtain porous fibrous material by electrostatic spinning apparatus；Porous fibre is soaked in dopamine solution and uniformly uploads poly-dopamine clad；Processed by high temperature cabonization, it is achieved the carbonization of the porous fibrous material that poly-dopamine is modified, uniformly upload two selenizing molybdenum nanometer sheet by hydro-thermal on porous fibre surface, prepare the porous carbon fiber/bis-selenizing molybdenum composite material based on poly-dopamine of uniqueness.Specifically comprise the following steps that
(1) spinnability macromolecule dissolution is configured to spinning liquid in solution, prepares porous fibre by the electrostatic spinning technique of Liquid acquisition device；
(2) porous fibre is placed in dopamine solution and reacts, obtain the clad of poly-dopamine；
(3) porous fibre that poly-dopamine is modified is carried out high temperature cabonization, obtain the carbon fibre material with loose structure；
(4) porous carbon fiber is soaked in concentrated acid solution 5-6h carries out acidification, then repeatedly washes 3-5 time with deionized water, drying for standby；
(5) being added in hydrazine hydrate by selenium simple substance, heating for dissolving is standby；
(6) by the carbon fiber of certain mass obtained above, put in solvent containing selenium simple substance hydrazine hydrate solution and molybdenum salt, be transferred in water heating kettle, in 180-220 DEG C of hydro-thermal reaction 12-24h；Porous carbon fiber/bis-selenizing molybdenum nanosheet composite material the deionized water obtained is washed 3-5 time repeatedly, then drying for standby；
(7) porous carbon fiber/bis-selenizing molybdenum nanosheet composite material prepared is carried out heat treatment and improve the crystal structure of two selenizing molybdenum nanometer sheet.
In the present invention, the spinnability macromolecule described in step (1) is selected from polyacrylonitrile, polyamic acid, polyamide and polystyrene, it is preferable that polystyrene；The spinning liquid range of solid content of configuration is 8% ~ 20%；Receive device institute holding liquid and include liquid nitrogen, ethanol.
In the present invention, the concentration range of the dopamine solution described in step (2) is 0.5 ~ 3mg/mL, wherein uses pH buffer Tris/Tris HCl, and its concentration is 10mM/L；Reaction temperature is 55-65 DEG C, and the response time is 3-12h.
In the present invention, high temperature cabonization process described in step (3) is: is placed in tube furnace by the porous fibre of obtained poly-dopamine cladding, controls temperature programming in nitrogen atmosphere, i.e. DEG C intensification from room temperature to 400-500, time is 1-2h, is incubated 0.5-1h；Then being warmed up to 600-800 ° of C again, the heating-up time is 1-3h, is incubated 1-2h, it is preferable that carburizing temperature is 700 DEG C ~ 800 DEG C.
In the present invention, the concentrated acid solution described in step (4) can be selected for: concentration more than 50% concentrated sulphuric acid or concentrated nitric acid solution.
In the present invention, the selenium simple substance described in step (5) is dissolved in hydrazine hydrate solution, and its concentration is 1 ~ 3mg/mL.
In the present invention, the molybdenum salt described in step (6) is selected from ammonium molybdate, sodium molybdate, ammonium thiomolybdate；Solvent used by disperse carbon fibers, molybdenum salt and selenium salt is selected from deionized water, ethanol, dimethyl acetylamide, N-Methyl pyrrolidone and dimethylformamide, it is preferable that deionized water.
In the present invention, the mol ratio of the molybdenum salt described in step (6) and selenium salt is 1:2, and the mass ratio that feeds intake of carbon fiber and two selenizing molybdenums is 4:1-4:4.
In the present invention, the heat treatment temperature described in step (7) is 300-450 DEG C, it is preferable that 340-380 DEG C.
Use SEM(scanning electron microscope), X-ray diffraction analysis, full-automatic adsorption instrument, electrochemical workstation characterize the structure and morphology of the porous carbon fiber/bis-selenizing molybdenum composite material that the present invention obtains and be used as the chemical property of electrochemical catalyst, its result is as follows:
(1) test result of SEM and BET shows: polystyrene (PS) has the spinnability of excellence.The present invention is prepared into porous PS fiber by the electric spinning equipment that ethanol receives, and obtains the porous carbon fiber of structure improvement after dopamine in-situ polymerization has the PSPDA fiber calcination of suitably poly-dopamine layer thickness.Its specific surface area is up to 378m2/ g, much larger than the pure carbon fiber (94m of solid construction2/ g).The aperture of fibrous inside pore structure is mainly distributed on 40-50nm, more consistent with observed result in SEM photograph, referring to accompanying drawing 2.If the poly-dopamine of cladding is very few, after high-temperature calcination, fibre structure is destroyed, and such as 2-CF, too much poly-dopamine clad then makes fiber surface poly-dopamine aggregate occur, such as 6-CF, sees accompanying drawing 3.Upload two selenizing molybdenum (MoSe further2) after, along with MoSe2The increase of precursor concentration, the MoSe that fiber is uploaded gradually2It is completely covered, and is affected by crystallization kinetics, MoSe2Nanoscale twins first reduces and increases and be perpendicular to gradually fiber surface distribution afterwards.Work as MoSe2Increase (MoSe to a certain extent2-CF-4/4), unnecessary MoSe2Trend towards in composite material surface autohemagglutination balling-up, referring to accompanying drawing 4.It was additionally observed that lamellar MoSe2Diameter be about 100nm and be approximately perpendicularly grown on the duct of fiber surface and fibrous inside, therefore it is considered that the high-specific surface area advantage of porous carbon fiber is fully used in this composite, referring to accompanying drawing 5.
(2) X-ray diffraction characterization result shows: occurs in that wider disperse peak at 25 ° and about 43 ° on the XRD of pure carbon fiber prepared in the present invention, represents that it is impalpable structure.And MoSe2-CF composite and pure MoSe2Particle is all in 2 θ=13.7 °, and 32.2 °, diffraction maximum occur in 37.3 ° and 56.4 ° of four positions, are respectively belonging to 2H-MoSe2(002), (100), (103) and (110) crystal face (JCPDS:87-2419).XRD is successfully authenticated MoSe from crystal formation2Successful upload on carbon fiber, referring to accompanying drawing 6.
(4) Electrochemical results shows: porous carbon fiber/bis-selenizing molybdenum composite material prepared in the present invention is a kind of good liberation of hydrogen catalyst, and pure carbon fiber is almost without hydrogen evolution activity, MoSe2Particle itself have activity but with carbon fiber compound after Hydrogen Evolution Performance be increased dramatically, the electrocatalytic hydrogen evolution of composite activity is along with MoSe2The increase of content first increases and reduces afterwards.MoSe2-CF-3/4 shows the electrocatalytic hydrogen evolution performance of optimum, and its initial overpotential is low to moderate 70mV, only higher about 40mV than business Pt/C, referring to accompanying drawing 7.
Visible, prepared by present invention porous carbon fiber/bis-selenizing molybdenum composite material, can as the electrode material of catalyst, hydrogen storage material and ultracapacitor or lithium ion battery.
The present invention has the remarkable advantages that:
(1) preparation process is gentle, environmental protection, it is easy to operation, is a kind of Green Chemistry preparation method；
(2) mentality of designing is ingenious: adopt the electric spinning equipment that ethanol receives to prepare porous PS fiber, is immersed in dopamine solution and obtains poly-dopamine clad.The carbonization utilizing removal and poly-dopamine that high-temperature burning process one step realizes template PS fiber obtains the porous carbon fiber of structure improvement；
(3) porous carbon fiber prepared by has higher specific surface area and higher electrical conductive activities, by it as MoSe2The matrix material of nanometer sheet growth, it is possible to effectively prevent MoSe2Nanometer sheet is reunited.
Accompanying drawing explanation
Fig. 1 is the preparation process schematic diagram of the carbon fiber loaded two selenizing molybdenum composite materials in hole, poly-dopamine Quito involved in the present invention.
Fig. 2 is the prepared pure carbon fiber 4-CF surface obtained based on poly-dopamine and sectional view, N in the present invention2Adsorption/desorption curve and pore size distribution curve.
The carbon fiber surface of the poly-dopamine thickness of difference that Fig. 3 is prepared in the present invention and sectional view: (a, b) 2-CF and (c, d) 6-CF.
Fig. 4 is different MoSe prepared in the present invention2-CF composite SEM schemes, wherein, and (a) MoSe2-CF-1/4, (b) MoSe2-CF-2/4, (c) MoSe2-CF-3/4 and (d) MoSe2-CF-4/4。
Fig. 5 is MoSe prepared in the present invention2The sectional view of-CF-1/4 composite.
Fig. 6 is the pure carbon fiber prepared by the present invention, MoSe2And MoSe2The XRD spectra of-CF-1/4 composite.
Fig. 7 is made pure carbon fiber, MoSe in the present invention2And MoSe2The linear scanning curve of-CF-1/4；Each MoSe2The linear sweep voltammetry curve of-CF composite and business Pt/C.
Detailed description of the invention
Below in conjunction with instantiation, the present invention is expanded on further, it should be appreciated that these embodiments are merely to illustrate the present invention rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, the present invention can be made various change or amendment by those skilled in the art, and these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
The present embodiment comprises the following steps:
(1) being dissolved in DMF by polystyrene PS and be configured to spinning liquid, the electrostatic spinning technique received by ethanol prepares PS porous fibre；
(2) PS porous fibre is placed in dopamine solution and reacts 4h, obtain the clad of poly-dopamine；
(3) the PS porous fibre that poly-dopamine is modified is carried out high temperature cabonization, obtain the carbon fibre material with loose structure, be designated as 4-CF；
(4) 4-CF is soaked in concentrated acid solution 5-6h carries out acidification, then repeatedly washes 3-5 time with deionized water, drying for standby；
(5) being added in hydrazine hydrate (3mg/mL) by selenium simple substance, heating for dissolving is standby；
(6) 20mg carbon fiber, 1mL are put in solvent containing selenium simple substance hydrazine hydrate solution and 4.76mg sodium molybdate, be transferred in water heating kettle, in 180-220 DEG C of hydro-thermal reaction 12-24h；Porous carbon fiber/bis-selenizing molybdenum nanosheet composite material the deionized water obtained is washed 3-5 time repeatedly, then drying for standby；
(7) porous carbon fiber/bis-selenizing molybdenum nanosheet composite material prepared is carried out heat treatment and improve the crystal structure of two selenizing molybdenum nanometer sheet, obtain product and be designated as MoSe2-CF-1/4。
Embodiment 2
Dopamine soak time in embodiment 1 is become 2h, and all the other are all with embodiment 1, and final obtained carbon fiber is designated as 2-CF, and excessively thin owing to being coated with poly-DOPA amine layer, after high-temperature calcination, fiber multihole is destructurized, referring to accompanying drawing 3.
Embodiment 3
Dopamine soak time in embodiment 1 is become 6h, and all the other are all with embodiment 1, and final obtained carbon fiber is designated as 6-CF, and too much poly-dopamine clad then makes fiber surface poly-dopamine aggregate occur, referring to accompanying drawing 3.
Embodiment 4
To become 2mL, 9.53mg containing selenium simple substance hydrazine hydrate solution and feeding intake of sodium molybdate in embodiment 1, all the other are all with embodiment 1, and final obtained composite is designated as MoSe2-CF-2/4, this material catalytic hydrogen evolution take-off potential is low to moderate 100mV (Vs.RHE).
Embodiment 5
To become 3mL, 14.28mg containing selenium simple substance hydrazine hydrate solution and feeding intake of sodium molybdate in embodiment 1, all the other are all with embodiment 1, and final obtained composite is designated as MoSe2-CF-3/4, this material catalytic hydrogen evolution take-off potential is low to moderate 70mV (Vs.RHE).
Embodiment 6
To become 4mL, 19.06mg containing selenium simple substance hydrazine hydrate solution and feeding intake of sodium molybdate in embodiment 1, all the other are all with embodiment 1, and final obtained composite is designated as MoSe2-CF-4/4, this material catalytic hydrogen evolution take-off potential is low to moderate 110mV (Vs.RHE).
In electro-chemical test, adopting three electrode test systems, with the platinum carbon electrode of prepared hybrid material modification for working electrode, saturated calomel electrode is reference electrode, and platinum filament is to electrode.Before testing, in advance by logical for electrolyte nitrogen 30min.Linear sweep voltammetry (LSV) is adopted to study the electrocatalytic hydrogen evolution reactivity of composite prepared in the present invention.Technological parameter relevant in above-mentioned electrochemical test method is as follows:
(1) pretreatment of platinum carbon electrode: platinum carbon electrode polishes with the alumina powder of 1.0,0.3,0.05 micron successively, makes into minute surface.Clean with deionized water and EtOH Sonicate after polishing every time, then dry up with nitrogen standby；
(2) preparation of modified electrode: adopt direct drop-coating to modify at the composite prepared by the surface present invention through the platinum carbon electrode of pretreatment.It is specially and prepared hybrid material is dispersed in deionized water and ethanol ratio for, in the solvent of 1:1, making the solution of 2mg/mL, after supersound process 1h, take 5 Al of Solution and drop on platinum carbon electrode, dry 0.5h in the baking oven of 70 DEG C.
Claims (11)
1. the preparation method based on the porous carbon fiber/bis-selenizing molybdenum composite material of poly-dopamine, it is characterised in that specifically comprise the following steps that
(1) spinnability macromolecule dissolution is configured to spinning liquid in solution, prepares porous fibre by the electrostatic spinning technique of Liquid acquisition device；
(2) porous fibre is placed in dopamine solution and reacts, obtain the clad of poly-dopamine；
(3) porous fibre that poly-dopamine is modified is carried out high temperature cabonization, obtain the carbon fibre material with loose structure；
(4) porous carbon fiber is soaked in concentrated acid solution 5-6h carries out acidification, then repeatedly washes 3-5 time with deionized water, drying for standby；
(5) being added in hydrazine hydrate by selenium simple substance, heating for dissolving is standby；
(6) by carbon fiber obtained above, put in solvent containing selenium simple substance hydrazine hydrate solution and molybdenum salt, be transferred in water heating kettle, in 180-220 DEG C of hydro-thermal reaction 12-24h；Porous carbon fiber/bis-selenizing molybdenum nanosheet composite material the deionized water obtained is washed 3-5 time repeatedly, then drying for standby；
(7) porous carbon fiber/bis-selenizing molybdenum nanosheet composite material prepared is carried out heat treatment and improve the crystal structure of two selenizing molybdenum nanometer sheet.
2. the preparation method of porous carbon fiber/bis-selenizing molybdenum composite material according to claim 1, it is characterised in that the spinnability macromolecule described in step (1) is selected from polyacrylonitrile, polyamic acid, polyamide and polystyrene；The spinning liquid range of solid content of configuration is 8% ~ 20%；Receive device institute holding liquid and include liquid nitrogen, ethanol.
3. the preparation method of porous carbon fiber/bis-selenizing molybdenum composite material according to claim 1 and 2, it is characterized in that the concentration range of the dopamine solution described in step (2) is 0.5 ~ 3mg/mL, wherein using pH buffer Tris/Tris HCl, its concentration is 10mM/L；Reaction temperature is 55-65 DEG C, and the response time is 3-12h.
4. the preparation method of porous carbon fiber/bis-selenizing molybdenum composite material according to claim 3, the high temperature cabonization process described in step (3) that it is characterized in that is: be placed in tube furnace by the porous fibre of obtained poly-dopamine cladding, nitrogen atmosphere controls temperature programming, i.e. DEG C intensification from room temperature to 400-500, time is 1-2h, is incubated 0.5-1h；Then being warmed up to 600-800 DEG C again, the heating-up time is 1-3h, is incubated 1-2h.
5. the preparation method of the porous carbon fiber/bis-selenizing molybdenum composite material according to claim 1,2 or 4, it is characterised in that the concentrated acid solution described in step (4) is concentration more than 50% concentrated sulphuric acid or concentrated nitric acid solution.
6. the preparation method of porous carbon fiber/bis-selenizing molybdenum composite material according to claim 5, it is characterised in that it is 1 ~ 3mg/mL that the selenium simple substance described in step (5) is dissolved in hydrazine hydrate solution compound concentration.
7. the preparation method of the porous carbon fiber/bis-selenizing molybdenum composite material according to claim 1,2,4 or 6, it is characterised in that the molybdenum salt described in step (6) is selected from ammonium molybdate, sodium molybdate, ammonium thiomolybdate；Solvent used by disperse carbon fibers, molybdenum salt and selenium salt is selected from deionized water, ethanol, dimethyl acetylamide, N-Methyl pyrrolidone and dimethylformamide.
8. the preparation method of porous carbon fiber/bis-selenizing molybdenum composite material according to claim 7, it is characterised in that the mol ratio of the molybdenum salt described in step (6) and selenium salt is 1:2, and the mass ratio that feeds intake of carbon fiber and two selenizing molybdenums is 4:1-4:4.
9. the preparation method of the porous carbon fiber/bis-selenizing molybdenum composite material according to claim 1,2,4,6 or 8, it is characterised in that the heat treatment temperature described in step (7) is 300-450 DEG C.
10. by the porous carbon fiber/bis-selenizing molybdenum composite material prepared according to the described preparation method of one of claim 1-9.
11. porous carbon fiber/bis-selenizing molybdenum composite material as claimed in claim 10 is as the application of catalyst, hydrogen storage material and ultracapacitor or the electrode material of lithium ion battery.
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