CN105742074B - Selenizing molybdenum composite material of a kind of porous carbon fiber based on poly-dopamine/bis- and preparation method thereof - Google Patents
Selenizing molybdenum composite material of a kind of porous carbon fiber based on poly-dopamine/bis- and preparation method thereof Download PDFInfo
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- CN105742074B CN105742074B CN201610199883.2A CN201610199883A CN105742074B CN 105742074 B CN105742074 B CN 105742074B CN 201610199883 A CN201610199883 A CN 201610199883A CN 105742074 B CN105742074 B CN 105742074B
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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
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Abstract
The invention belongs to complex fiber material technical field, selenizing molybdenum nanosheet composite material of specially a kind of porous carbon fiber based on poly-dopamine/bis- and preparation method thereof.The method of the present invention includes:Spinnability high molecular material is configured to spinning solution, the uniform porous fibre of structure is prepared by electrostatic spinning apparatus;Porous fibre is soaked in dopamine solution, the thickness of poly-dopamine clad is controlled by the concentration and reaction time that adjust dopamine solution;It is handled by high temperature cabonization, realizes the carbonization of the porous fibrous material of poly-dopamine modification;By hydro-thermal two selenizing molybdenum nanometer sheets are uniformly uploaded on porous fibre surface.The advantages that the method for the present invention safety and environmental protection, the active content of material of the selenizing molybdenum of the porous carbon fiber prepared/bis- are high, specific surface area is high, conductivity is high and physical and chemical performance is stablized is the ideal electrode material for preparing active elctro-catalyst for evolving hydrogen reaction.
Description
Technical field
The invention belongs to complex fiber material technical fields, and in particular to a kind of selenizing molybdenum composite wood of porous carbon fiber/bis-
Material and preparation method thereof.
Background technology
Nanofiber is the Typical Representative of monodimension nanometer material, and electrostatic spinning technique directly can continuously be made as one kind
The method of standby polymer nanofiber, is widely noticed all the time.The nano fibrous membrane being prepared because it is good with stability,
It the advantages that porosity height, large specific surface area, conductivity height and more substance and electron-transport duct, can be widely applied to be catalyzed
The electrode material etc. of agent carrier, hydrogen storage material, sorbing material and ultracapacitor or lithium ion battery, advantageously accounts for current society
The energy crisis and problem of environmental pollution of meeting.
Traditional electrostatic spinning nano fiber surface is smooth, and structure is single, it is difficult to meet the needs of practical application.Porous structure
Introducing, increase the specific surface area of fibrous material, be also conducive to improve material surface-active.Present invention firstly provides based on
The preparation method of the porous structure carbon fibre material of poly-dopamine, it is intended to pass through this novel fiber with multi-stage pore structure
The preparation of material can make up the deficiency of traditional fibre material, to be applied in more areas.
Two selenizing molybdenums(MoSe2)For a kind of two-dimentional Transition-metal dichalcogenide with graphite-like structure.In its single layer
Se atoms and Mo atoms are tightly packed at " Se-Mo-Se " sandwich type structural by three layers of covalent bond form, and interlayer passes through Van der Waals
Power interacts.The Se atoms and Mo atoms that the interlayer structure of this type graphite makes to leak outside cruelly have good chemism.
Porous carbon fiber material is prepared in present invention combination electrostatic spinning technique and the self-polymeric reaction of poly-dopamine.Utilize solvent-thermal method
MoSe is grown in porous fibre surface in situ2Nanoscale twins are successfully realized one-dimensional porous carbon fiber and two dimension MoSe2Nanometer sheet
The controllable of layer multilevel hierarchy composite material is constructed.The composite material has following advantage:It is prepared based on the more of poly-dopamine
Pore structure carbon fiber has larger specific surface area, using it as MoSe2The basis material of nanometer sheet growth, can effectively prevent
Only MoSe2Nanometer sheet is reunited;Furthermore the porous structure carbon fiber based on poly-dopamine have excellent electric conductivity, be conducive to from
The quick transmission of son and electronics, MoSe2With excellent catalytic performance and higher capacity and energy density, the two is had
Constructing for effect, can maximize favourable factors and minimize unfavourable ones, effectively play respective advantage.
Invention content
Novel porous carbon fiber/bis- that the purpose of the present invention is to provide a kind of preparation process is simple, manufacturing cost is cheap
Selenizing molybdenum composite material and preparation method thereof.
The selenizing molybdenum composite material of porous carbon fiber provided by the present invention/bis-, preparing raw material composition includes:High score can be spun
Son, dopamine, selenium simple substance, molybdenum salt.
The selenizing molybdenum composite material of porous carbon fiber provided by the present invention/bis-, selection Static Spinning porous fibre are substrate, are led to
It crosses the oxidation self-polymeric reaction of dopamine and the last hydro-thermal of high temperature cabonization process is uploaded two selenizing molybdenums and is prepared.
The present invention is to provide a kind of high-specific surface area, high porosity, the porous knots being carbonized by poly-dopamine shell
The carbon fiber loaded two selenizings molybdenum composite material of structure.
The selenizing molybdenum composite material of porous carbon fiber provided by the present invention/bis-, preparation process include:Pass through electrostatic spinning
Device obtains porous fibrous material;Porous fibre is soaked in dopamine solution and uniformly uploads poly-dopamine clad;Pass through
The carbonization of the porous fibrous material of poly-dopamine modification is realized in high temperature cabonization processing, uniform on porous fibre surface by hydro-thermal
Two selenizing molybdenum nanometer sheets are uploaded, the selenizing molybdenum composite material of the unique porous carbon fiber based on poly-dopamine/bis- is prepared.Specifically
Steps are as follows:
(1)Spinnability macromolecule dissolution is configured to spinning solution in solution, passes through the electrostatic spinning of Liquid acquisition device
Porous fibre is prepared in technology;
(2)Porous fibre is placed in dopamine solution and is reacted, the clad of poly-dopamine is obtained;
(3)The porous fibre of poly-dopamine modification is subjected to high temperature cabonization, obtains the carbon fibre material with porous structure;
(4)Porous carbon fiber is soaked in 5-6 h in concentrated acid solution and carries out acidification, is then washed repeatedly with deionized water
3-5 times, drying for standby;
(5)Selenium simple substance is added in hydrazine hydrate, is dissolved by heating spare;
(6)The carbon fiber of certain mass obtained above, the hydrazine hydrate solution of simple substance containing selenium and molybdenum salt are put into solvent, turned
It moves in water heating kettle, in 180-220 DEG C of hydro-thermal reaction 12-24 h;The selenizing molybdenum nanometer sheet of obtained porous carbon fiber/bis- is answered
Condensation material is washed 3-5 times repeatedly with deionized water, then drying for standby;
(7)The selenizing molybdenum nanosheet composite material of the porous carbon fiber being prepared/bis- is subjected to heat treatment and improves two selenizings
The crystal structure of molybdenum nanometer sheet.
In the present invention, step(1)Described in spinnability macromolecule be selected from polyacrylonitrile, polyamic acid, polyamide and
Polystyrene, preferably polystyrene;The spinning solution range of solid content of configuration is 8% ~ 20%;Reception device institute holding liquid includes liquid
Nitrogen, ethyl alcohol.
In the present invention, step(2)Described in dopamine solution concentration range be 0.5 ~ 3 mg/mL, wherein use pH
Buffer solution Tris/TrisHCl, a concentration of 10 mM/L;Reaction temperature is 55-65 DEG C, and the reaction time is 3-12 h.
In the present invention, step(3)Described in high temperature cabonization process be:The porous fibre that obtained poly-dopamine is coated
Dimension is placed in tube furnace, and temperature programming is controlled in nitrogen atmosphere, i.e., from room temperature to 400-500 DEG C, the time is 1-2 h,
Keep the temperature 0.5-1 h;Then it is warming up to 600-800 °C again, the heating-up time is 1-3 h, keeps the temperature 1-2 h, and preferably carburizing temperature is
700℃ ~800℃。
In the present invention, step(4)Described in concentrated acid solution can be selected:50% or more the concentrated sulfuric acid of concentration or concentrated nitric acid are molten
Liquid.
In the present invention, step(5)Described in selenium simple substance be dissolved in hydrazine hydrate solution, a concentration of 1 ~ 3 mg/mL.
In the present invention, step(6)Described in molybdenum salt be selected from ammonium molybdate, sodium molybdate, ammonium thiomolybdate;Disperse carbon fibers,
Solvent used in molybdenum salt and selenium salt is selected from deionized water, ethyl alcohol, dimethylacetylamide, N-Methyl pyrrolidone and dimethyl formyl
Amine, preferably deionized water.
In the present invention, step(6)The molar ratio of the molybdenum salt and selenium salt is 1:2, carbon fiber feeds intake with two selenizing molybdenums
Mass ratio is 4:1-4:4.
In the present invention, step(7)The heat treatment temperature is 300-450 DEG C, preferably 340-380 DEG C.
Use SEM(Scanning electron microscope), X-ray diffraction analysis, automatic adsorption device, electrochemical workstation carry out table
The structure and morphology of the selenizing molybdenum composite material of the porous carbon fiber that the sign present invention is obtained/bis- and electrification as electrochemical catalyst
Performance is learned, result is as follows:
(1)The test result of SEM and BET shows:Polystyrene(PS)With excellent spinnability.The present invention passes through ethyl alcohol
The electric spinning equipment of reception is prepared into porous PS fibers, has the PS@of appropriate poly-dopamine layer thickness by dopamine in-situ polymerization
Structurally consummate porous carbon fiber is obtained after PDA fiber calcinations.Its specific surface area is up to 378m2/ g is much larger than solid construction
Pure carbon fiber(94 m2/g).The aperture of fibrous inside pore structure is mainly distributed on 40-50 nm, is tied with being observed in SEM photograph
Fruit is more consistent, referring to attached drawing 2.If the poly-dopamine of cladding is very few, fibre structure is destroyed after high-temperature calcination, such as 2-CF, excessively
Poly-dopamine clad so that fiber surface poly-dopamine aggregate, such as 6-CF is occurred, see attached drawing 3.Further upload two selenium
Change molybdenum(MoSe2)Afterwards, with MoSe2The increase of precursor concentration, the MoSe being gradually uploaded on fiber2It is completely covered, and is tied
Brilliant kinetic effect, MoSe2Nanoscale twins first reduce to be increased and is gradually distributed perpendicular to fiber surface afterwards.Work as MoSe2Increase to one
Determine degree(MoSe2-CF-4/4), extra MoSe2It is intended in composite material surface autohemagglutination balling-up, referring to attached drawing 4.Also observe
To sheet MoSe2Diameter be about 100 nm and be approximately perpendicularly grown in 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 material, referring to attached drawing 5.
(2)X-ray diffraction characterization result shows:At 25 ° and 43 ° on the XRD of prepared pure carbon fiber in the present invention
There is wider disperse peak in left and right, indicates that it is impalpable structure.And MoSe2- CF composite materials and pure MoSe2Particle is 2
There is diffraction maximum, are respectively belonging to 2H-MoSe in θ=13.7 °, 32.2 °, 37.3 ° and 56.4 ° four positions2's(002)、
(100)、(103)With(110)Crystal face (JCPDS: 87-2419).XRD is successfully authenticated MoSe from crystal form2On carbon fiber
Successful upload, referring to attached drawing 6.
(4)Electrochemical results show:The selenizing molybdenum composite material of prepared porous carbon fiber in the present invention/bis- is one
The good liberation of hydrogen catalyst of kind, pure carbon fiber is almost without hydrogen evolution activity, MoSe2Particle itself is active but compound with carbon fiber
Hydrogen Evolution Performance is increased dramatically later, and the electrocatalytic hydrogen evolution activity of composite material is with MoSe2After the increase of content first increases
Reduce.MoSe2- CF-3/4 shows optimal electrocatalytic hydrogen evolution performance, and starting overpotential is down to 70 mV, only than business Pt/
40 mV of C high or so, referring to attached drawing 7.
As it can be seen that porous carbon fiber/bis- selenizing molybdenum composite material prepared by the present invention, can be used as catalyst, hydrogen storage material and
The electrode material of ultracapacitor or lithium ion battery.
The present invention remarkable advantage be:
(1)Preparation process is mild, environmentally friendly, easily operated, is a kind of Green Chemistry preparation method;
(2)Mentality of designing is ingenious:Porous PS fibers are prepared in the electric spinning equipment received using ethyl alcohol, are immersed in more
Poly-dopamine clad is obtained in bar amine aqueous solution.The removal of template PS fibers is realized using one step of high-temperature burning process and is gathered more
The carbonization of bar amine obtains structurally consummate porous carbon fiber;
(3)Prepared porous carbon fiber has higher specific surface area and higher electrical conductive activities, using it as MoSe2
The basis material of nanometer sheet growth, can effectively prevent MoSe2Nanometer sheet is reunited.
Description of the drawings
Fig. 1 is the preparation of the carbon fiber loaded two selenizings molybdenum composite material in poly-dopamine Quito hole involved in the present invention
Journey schematic diagram.
Fig. 2 is the surfaces pure carbon fiber 4-CF obtained based on poly-dopamine and sectional view prepared in the present invention, N2It inhales
Attached desorption curve and pore size distribution curve.
Fig. 3 is the carbon fiber surface and sectional view of different poly-dopamine thickness prepared in the present invention:(a, b)2-CF
With(c, d)6-CF.
Fig. 4 is different MoSe prepared in the present invention2- CF composite materials SEM figures, wherein(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 materials.
Fig. 6 is pure carbon fiber prepared in the present invention, MoSe2And MoSe2The XRD spectra of-CF-1/4 composite materials.
Fig. 7 is made pure carbon fiber, MoSe in the present invention2And MoSe2The linear scan curve of-CF-1/4;Each MoSe2-
The linear sweep voltammetry curve of CF composite materials and business Pt/C.
Specific implementation mode
With reference to specific example, the present invention is further explained, it should be appreciated 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, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Various changes or modification can be made to the present invention, such equivalent forms are equally fallen within defined by the application the appended claims
Range.
Embodiment 1
The present embodiment includes the following steps:
(1)Polystyrene PS is dissolved in DMF and is configured to spinning solution, is prepared by the electrostatic spinning technique that ethyl alcohol receives
Obtain PS porous fibres;
(2)PS porous fibres are placed in dopamine solution and react 4 h, obtain the clad of poly-dopamine;
(3)The PS porous fibres of poly-dopamine modification are subjected to high temperature cabonization, obtain the carbon fiber material with porous structure
Material, is denoted as 4-CF;
(4)4-CF is soaked in 5-6 h in concentrated acid solution and carries out acidification, is then washed 3-5 times repeatedly with deionized water,
Drying for standby;
(5)Selenium simple substance is added in hydrazine hydrate(3 mg/mL), dissolve by heating spare;
(6)20 mg carbon fibers, 1 mL simple substance containing selenium hydrazine hydrate solution and 4.76 mg sodium molybdates are put into solvent, are shifted
Into water heating kettle, in 180-220 DEG C of hydro-thermal reaction 12-24 h;Obtained porous carbon fiber/bis- selenizing molybdenum nanometer sheets are compound
Material is washed 3-5 times repeatedly with deionized water, then drying for standby;
(7)The selenizing molybdenum nanosheet composite material of the porous carbon fiber being prepared/bis- is subjected to heat treatment and improves two selenizings
The crystal structure of molybdenum nanometer sheet obtains product and is denoted as MoSe2-CF-1/4。
Embodiment 2
Dopamine soaking time in embodiment 1 is become into 2 h, remaining is with embodiment 1, the carbon fiber that is finally obtained
It is denoted as 2-CF, since cladding poly-dopamine layer is excessively thin, fiber multihole is destructurized after high-temperature calcination, referring to attached drawing 3.
Embodiment 3
Dopamine soaking time in embodiment 1 is become into 6 h, remaining is with embodiment 1, the carbon fiber that is finally obtained
It is denoted as 6-CF, excessive poly-dopamine clad then makes fiber surface poly-dopamine aggregate occur, referring to attached drawing 3.
Embodiment 4
By in embodiment 1 the hydrazine hydrate solution of simple substance containing selenium and feeding intake for sodium molybdate become 2 mL, 9.53 mg, remaining
With embodiment 1, the composite material finally obtained is denoted as MoSe2- CF-2/4, the material catalytic hydrogen evolution take-off potential is down to 100
mV(Vs. RHE)。
Embodiment 5
By in embodiment 1 the hydrazine hydrate solution of simple substance containing selenium and feeding intake for sodium molybdate become 3 mL, 14.28 mg, remaining
With embodiment 1, the composite material finally obtained is denoted as MoSe2- CF-3/4, the material catalytic hydrogen evolution take-off potential is down to 70
mV(Vs. RHE)。
Embodiment 6
By in embodiment 1 the hydrazine hydrate solution of simple substance containing selenium and feeding intake for sodium molybdate become 4 mL, 19.06 mg, remaining
With embodiment 1, the composite material finally obtained is denoted as MoSe2- CF-4/4, the material catalytic hydrogen evolution take-off potential is down to 110
mV(Vs. RHE)。
In electro-chemical test, using three electrode test systems, it is with the platinum carbon electrode that prepared hybrid material is modified
Working electrode, saturated calomel electrode are reference electrode, and platinum filament is to electrode.Before testing, electrolyte is led into nitrogen 30 in advance
min.Using linear sweep voltammetry(LSV)The electrocatalytic hydrogen evolution reactivity of prepared composite material in the research present invention.
Relevant technological parameter is as follows in above-mentioned electrochemical test method:
(1)The pretreatment of platinum carbon electrode:Platinum carbon electrode is polished with 1.0,0.3,0.05 microns of alumina powder successively, is made
At minute surface.It is cleaned, is then dried up with nitrogen spare with deionized water and EtOH Sonicate after polishing every time;
(2)The preparation of modified electrode:Using direct drop-coating in the surface present invention by pretreated platinum carbon electrode
Prepared composite material is modified.It is 1 that prepared hybrid material, which is specially dispersed in deionized water and ethyl alcohol ratio,:1
Solvent in, be made the solution of 2 mg/mL, after being ultrasonically treated 1 h, take 5 microlitres of solution to drop on platinum carbon electrode, in 70 DEG C of baking
Dry 0.5 h in case.
Claims (11)
1. a kind of porous carbon fiber based on poly-dopamine/bis- selenizing molybdenum composite material preparation method, it is characterised in that it is specific
Steps are as follows:
(1)Spinnability macromolecule dissolution is configured to spinning solution in solution, passes through the electrostatic spinning equipped with Liquid acquisition device
Porous fibre is prepared in technology;
(2)Porous fibre is placed in dopamine solution and is reacted, the clad of poly-dopamine is obtained;
(3)The porous fibre of poly-dopamine modification is subjected to high temperature cabonization, obtains the carbon fibre material with porous structure;
(4)Porous carbon fiber is soaked in 5-6 h in concentrated acid solution and carries out acidification, then washes 3-5 repeatedly with deionized water
It is secondary, drying for standby;
(5)Selenium simple substance is added in hydrazine hydrate, is dissolved by heating spare;
(6)Carbon fiber obtained above, the hydrazine hydrate solution of simple substance containing selenium and molybdenum salt are put into solvent, are transferred in water heating kettle,
In 180-220 DEG C of hydro-thermal reaction 12-24 h;By the selenizing molybdenum nanosheet composite material deionization of obtained porous carbon fiber/bis-
Water is washed 3-5 times repeatedly, then drying for standby;
(7)The selenizing molybdenum nanosheet composite material of the porous carbon fiber being prepared/bis- be subjected to heat treatment improve two selenizing molybdenums to receive
The crystal structure of rice piece.
2. porous carbon fiber according to claim 1/bis- selenizing molybdenum composite material preparation method, it is characterised in that step
(1)Described in spinnability macromolecule be selected from polyacrylonitrile, polyamic acid, polyamide and polystyrene;The spinning solution of configuration
Range of solid content is 8% ~ 20%;Reception device institute holding liquid includes liquid nitrogen or ethyl alcohol.
3. porous carbon fiber according to claim 1 or 2/bis- selenizing molybdenum composite material preparation method, it is characterised in that
Step(2)Described in dopamine solution concentration range be 0.5 ~ 3 mg/mL, wherein use pH buffer solutions Tris/Tris
HCl, a concentration of 10 mM/L;Reaction temperature is 55-65 DEG C, and the reaction time is 3-12 h.
4. porous carbon fiber according to claim 3/bis- selenizing molybdenum composite material preparation method, it is characterised in that step
(3)Described in high temperature cabonization process be:The porous fibre that obtained poly-dopamine coats is placed in tube furnace, in nitrogen
Temperature programming is controlled in atmosphere, i.e., from room temperature to 400-500 DEG C, the time is 1-2 h, heat preservation 0.5-1 h;Then it heats up again
To 600-800 DEG C, the heating-up time is 1-3 h, heat preservation 1-2 h.
5. porous carbon fiber according to claim 1,2 or 4/bis- selenizing molybdenum composite material preparation method, feature exists
In step(4)Described in concentrated acid solution be 50% or more the concentrated sulfuric acid of concentration or concentrated nitric acid solution.
6. porous carbon fiber according to claim 5/bis- selenizing molybdenum composite material preparation method, it is characterised in that step
(5)Described in selenium simple substance be dissolved in hydrazine hydrate solution compound concentration be 1 ~ 3 mg/mL.
7. porous carbon fiber according to claim 1,2,4 or 6/bis- selenizing molybdenum composite material preparation method, feature
It is step(6)Described in molybdenum salt be selected from ammonium molybdate, sodium molybdate, ammonium thiomolybdate;Used in disperse carbon fibers, molybdenum salt and selenium salt
Solvent be selected from deionized water, ethyl alcohol, dimethylacetylamide, N-Methyl pyrrolidone and dimethylformamide.
8. porous carbon fiber according to claim 7/bis- selenizing molybdenum composite material preparation method, it is characterised in that step
(6)Described in the molar ratio of molybdenum salt and selenium salt be 1:2, the mass ratio that feeds intake of carbon fiber and two selenizing molybdenums is 4:1-4:4.
9. porous carbon fiber according to claim 1,2,4,6 or 8/bis- selenizing molybdenum composite material preparation method, it is special
Sign is step(7)The heat treatment temperature is 300-450 DEG C.
10. by the porous carbon fiber/bis- selenizing molybdenum composite wood being prepared according to one of the claim 1-9 preparation methods
Material.
11. porous carbon fiber as claimed in claim 10/bis- selenizing molybdenum composite material as catalyst, hydrogen storage material and super
The application of the electrode material of capacitor or lithium ion battery.
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