CN106784745A - The sodium-ion battery method for manufacturing electric spinning of cobaltosic oxide carbon nano-fiber - Google Patents
The sodium-ion battery method for manufacturing electric spinning of cobaltosic oxide carbon nano-fiber Download PDFInfo
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Abstract
Sodium-ion battery Co3O4The method for manufacturing electric spinning of carbon nano-fiber, with Co2+Salt, polyvinylpyrrolidone and organic solvent composition Electrospun precursor liquid, Co is prepared using electrical spinning method2+Salt/PVP composite cellulosic membranes, then, Co processed is obtained by air atmosphere calcine technology3O4Carbon nano-fiber, the Co of preparation3O4Crystal has regular hexagonal nano sheet structure, and be equably embedded in carbon nano-fiber, so that material has larger specific surface area, unique carbon nano-fiber loose structure and ultrathin nanometer piece cross-linked structure, it is effectively facilitated the infiltration of electrolyte and the transfer of electrons/ions, shorten sodium ion diffusion path in the material, be conducive to the insertion and deintercalation of sodium ion, with capacitance and preferable cyclical stability higher, substantially increase the dynamic performance of material, the process is simple of the invention, low cost.
Description
Technical field
The invention belongs to anode material of lithium-ion battery technical field, and in particular to sodium-ion battery Co3O4Carbon Nanowire
The method for manufacturing electric spinning of dimension.
Background technology
Past many decades, lithium ion battery is with its energy density higher and service life more long all kinds of portable
It is used widely in electronic equipment, electric motor car.It is expensive but lithium resource is limited, lithium ion is limited to a certain extent
The large-scale application of battery.Sodium is in same main group with lithium in the periodic table of elements, with similar physicochemical properties.Sodium from
Sub- battery is because sodium resource reserves are abundant, environment-friendly receive extensive concern.The research and development of sodium-ion battery are certain
Can be relaxed in degree because the battery that lithium resource shortage triggers develops limitation problem, it is considered to be substitute lithium ion battery as big rule
Ideal chose of the mould energy-accumulating power station with stand-by power source and electric powered motor power supply of future generation.However, because the radius of sodium ion will
Bigger than the radius of lithium ion by 55%, sodium ion diffusion velocity is slow in causing electrochemical reaction process, it is difficult to embedded and deintercalation is in
Through commercialized graphite as anode material for lithium-ion battery powder.Suitable anode material of lithium-ion battery is thus found as sodium ion
The focus of battery research.
In past more than ten year, researcher has carried out extensive research to the positive electrode of sodium-ion battery,
But the research to anode material of lithium-ion battery is still at an early stage.In existing anode material of lithium-ion battery system,
Carbon nano-fiber has good impulse electricity cyclical stability, but its reversible specific capacity is too low (less than 300mAhg-1), it is impossible to it is full
The demand of sufficient height ratio capacity sodium-ion battery commercial applications.Existing result of study shows that transition metal oxide is used as sodium
Ion battery cathode material has theoretical reversible specific capacity (about 1000mAhg very high-1).Rahman M.M. et al.
(Chem.Commun., 50 (2014) 5057-5060) report Co3O4Powder as anode material of lithium-ion battery research knot
Really：In 25mAg-1Current density under, circulation 50 times after, its reversible specific capacity remains at 447mAhg-1.But due to Co3O4
Electrons/ions electrical conductivity itself is relatively low, so as to reduce its high rate performance as electrode material, along with its complicated electrode
Manufacturing process, limits its large-scale use as anode material of lithium-ion battery.
The content of the invention
In order to overcome the shortcoming of above-mentioned prior art, object of the present invention is to provide sodium-ion battery Co3O4Carbon is received
The method for manufacturing electric spinning of rice fiber, the Co of preparation3O4Carbon nano-fiber is by Co3O4Reversible specific capacity higher and carbon Nanowire
The electrons/ions electrical conductivity higher of dimension combines, and has the advantages that process is simple, low cost.
In order to achieve the above object, the technical scheme taken of the present invention is：
Sodium-ion battery Co3O4The method for manufacturing electric spinning of carbon nano-fiber, comprises the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 it is mixed
In conjunction solution, Co2+The quality of salt is 0.14~0.29g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Then polyvinylpyrrolidone (PVP) powder is added to mixed solution again, stirring obtains uniform Electrospun precursor liquid, poly- second
Alkene pyrrolidone (PVP) is 0.08~0.15g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is selected from any one in cobalt chloride, cobalt nitrate or cobaltous sulfate；
Described organic solvent is selected from any one in ethanol, methyl alcohol or N,N-dimethylformamide (DMF)；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carry out it is quiet
Electrospun, obtains Co2+Salt/PVP composite cellulosic membranes, 12~25kV of spinning voltage；Spacing 8~20cm of the shower nozzle to receiver board；Ring
Border humidity 30~60%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and are made
Its pre-oxidation and carbonization, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 0.5~6 DEG C/min；Calcining heat is 300~400 DEG C；Calcination time is
2~5h；Calcination atmosphere is air；
The parameter of carbonization is：Heating rate is 3~8 DEG C/min；Calcining heat is 700~900 DEG C；Calcination time be 2~
5h；Calcination atmosphere is air.
According to Co prepared by the above method3O4Carbon nano-fiber, its Co3O4The pattern of nanocrystal is ultra-thin hexagonal nano
Sheet, particle diameter is 5~20nm, is equably embedded in the diameter about carbon nano-fiber of 150nm, Co3O4Carbon nano-fiber is used for sodium
Ion battery cathode material.
Beneficial effects of the present invention are：The present invention utilizes electrical spinning method and air atmosphere calcine technology, prepares sodium ion electricity
Pond Co3O4Carbon nano-fiber negative material, further improves Co3O4Carbon nano-fiber specific surface area.The Co of preparation3O4Carbon nanometer
Fiber is crosslinked mosaic texture between having unique ultrathin nanometer piece and porous carbon nanofiber, is effectively facilitated oozing for electrolyte
The transfer of saturating and electrons/ions, shortens sodium ion diffusion path in the material, is conducive to the insertion and deintercalation of sodium ion.
100mAg-1Current density under, its reversible specific capacity that discharges first can reach 654mAhg-1, after circulating 60 times, its reversible specific volume
Amount is maintained at 518mAhg-1, there is preferable capability retention and preferable cyclical stability under high current density, answered
There is excellent charge-discharge magnification performance for sodium-ion battery negative pole, the application of sodium-ion battery Large Copacity energy stores is met
Demand, has the advantages that process is simple, low cost.
Brief description of the drawings
Fig. 1 (a) and Fig. 1 (b) are the SEM images of presoma nanofiber in embodiment 1；Fig. 1 (c) and (d) are embodiments 1
The Co of preparation3O4The SEM image of carbon nano-fiber.
Fig. 2 is Co prepared by embodiment 13O4Carbon nano-fiber is in 100mAg-1Current density under cycle performance figure.
Specific embodiment
The present invention is described in detail with reference to embodiments.
Embodiment 1, sodium-ion battery Co3O4The method for manufacturing electric spinning of carbon nano-fiber, comprises the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 it is mixed
In conjunction solution, Co2+The quality of salt is 0.14g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then again
Polyvinylpyrrolidone (PVP) powder is added to mixed solution, stirring obtains uniform Electrospun precursor liquid, polyvinyl pyrrole
Alkanone (PVP) is 0.08g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is cobalt nitrate；
Described organic solvent is ethanol；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carry out it is quiet
Electrospun, obtains Co2+Salt/PVP composite cellulosic membranes, spinning voltage 15kV；Spacing 12cm of the shower nozzle to receiver board；Ambient humidity
50%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and are made
Its pre-oxidation and carbonization, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 2 DEG C/min；Calcining heat is 350 DEG C；Calcination time is 2h；Calcining gas
Atmosphere is air；
The parameter of carbonization is：Heating rate is 4 DEG C/min；Calcining heat is 800 DEG C；Calcination time is 2h；Calcination atmosphere
It is air.
Fig. 1 (a) and (b) are the Co of the present embodiment2+The SEM image of salt/PVP composite cellulosic membranes, is combined as can be seen from Figure
Tunica fibrosa has and smooth shows pattern；Fig. 1 (c) and (d) are the present embodiment Co3O4The SEM image of carbon nano-fiber, from figure
Can be seen that such material to have between the ultrathin nanometer piece and porous carbon nanofiber of uniqueness to be crosslinked mosaic texture, can effectively facilitate
The infiltration of electrolyte and the transfer of electrons/ions, shorten sodium ion diffusion path in the material, are conducive to the insertion of sodium ion
And deintercalation.
Fig. 2 is the present embodiment Co3O4Carbon nano-fiber, in 100mAg-1Current density under cycle performance figure, can from figure
Find out that the material reversible specific capacity that discharges first can reach 654mAhg-1, after circulating 60 times, its reversible specific capacity is maintained at
518mAhg-1, show Co3O4Carbon nano-fiber negative material under high current density have preferable capability retention and preferably
Cyclical stability, being applied to sodium-ion battery negative pole has excellent charge-discharge magnification performance.
Embodiment 2, sodium-ion battery Co3O4The method for manufacturing electric spinning of carbon nano-fiber, comprises the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 it is mixed
In conjunction solution, Co2+The quality of salt is 0.16g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then again
Polyvinylpyrrolidone (PVP) powder is added to mixed solution, stirring obtains uniform Electrospun precursor liquid, polyvinyl pyrrole
Alkanone (PVP) is 0.10g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is cobalt chloride；
Described organic solvent is methyl alcohol；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carry out it is quiet
Electrospun, obtains Co2+Salt/PVP composite cellulosic membranes, spinning voltage 12kV；Spacing 8cm of the shower nozzle to receiver board；Ambient humidity
35%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and are made
Its pre-oxidation and carbonization, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 1 DEG C/min；Calcining heat is 300 DEG C；Calcination time is 2.5h；Calcining
Atmosphere is air；
The parameter of carbonization is：Heating rate is 4 DEG C/min；Calcining heat is 700 DEG C；Calcination time is 2.5h；Calcining gas
Atmosphere is air.
The present embodiment Co3O4Carbon nano-fiber is in 100mAg-1Current density under cycle performance and embodiment 1 it is close,
Show Co3O4Carbon nano-fiber negative material has preferable capability retention and preferable stable circulation under high current density
Property, being applied to sodium-ion battery negative pole has excellent charge-discharge magnification performance.
Embodiment 3, sodium-ion battery Co3O4The method for manufacturing electric spinning of carbon nano-fiber, comprises the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 it is mixed
In conjunction solution, Co2+The quality of salt is 0.18g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then again
Polyvinylpyrrolidone (PVP) powder is added to mixed solution, stirring obtains uniform Electrospun precursor liquid, polyvinyl pyrrole
Alkanone (PVP) is 0.12g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is cobaltous sulfate；
Described organic solvent is N,N-dimethylformamide (DMF)；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carry out it is quiet
Electrospun, obtains Co2+Salt/PVP composite cellulosic membranes, spinning voltage 18kV；Spacing 10cm of the shower nozzle to receiver board；Ambient humidity
30%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and are made
Its pre-oxidation and carbonization, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 0.5 DEG C/min；Calcining heat is 320 DEG C；Calcination time is 3h；Calcining
Atmosphere is air；
The parameter of carbonization is：Heating rate is 3 DEG C/min；Calcining heat is 750 DEG C；Calcination time is 3h；Calcination atmosphere
It is air.
The present embodiment Co3O4Carbon nano-fiber is in 100mAg-1Current density under cycle performance and embodiment 1 it is close,
Show Co3O4Carbon nano-fiber negative material has preferable capability retention and preferable stable circulation under high current density
Property, being applied to sodium-ion battery negative pole has excellent charge-discharge magnification performance.
Embodiment 4, sodium-ion battery Co3O4The method for manufacturing electric spinning of carbon nano-fiber, comprises the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 it is mixed
In conjunction solution, Co2+The quality of salt is 0.20g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then again
Polyvinylpyrrolidone (PVP) powder is added to mixed solution, stirring obtains uniform Electrospun precursor liquid, polyvinyl pyrrole
Alkanone (PVP) is 0.13g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is cobalt chloride；
Described organic solvent is ethanol；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carry out it is quiet
Electrospun, obtains Co2+Salt/PVP composite cellulosic membranes, spinning voltage 25kV；Spacing 20cm of the shower nozzle to receiver board；Ambient humidity
40%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and are made
Its pre-oxidation and carbonization, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 3 DEG C/min；Calcining heat is 360 DEG C；Calcination time is 5h；Calcining gas
Atmosphere is air；
The parameter of carbonization is：Heating rate is 5 DEG C/min；Calcining heat is 800 DEG C；Calcination time is 5h；Calcination atmosphere
It is air.
The present embodiment Co3O4Carbon nano-fiber is in 100mAg-1Current density under cycle performance and embodiment 1 it is close,
Show Co3O4Carbon nano-fiber negative material has preferable capability retention and preferable stable circulation under high current density
Property, being applied to sodium-ion battery negative pole has excellent charge-discharge magnification performance.
Embodiment 5, sodium-ion battery Co3O4The method for manufacturing electric spinning of carbon nano-fiber, comprises the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 it is mixed
In conjunction solution, Co2+The quality of salt is 0.26g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then again
Polyvinylpyrrolidone (PVP) powder is added to mixed solution, stirring obtains uniform Electrospun precursor liquid, polyvinyl pyrrole
Alkanone (PVP) is 0.13g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is cobaltous sulfate；
Described organic solvent is methyl alcohol；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carry out it is quiet
Electrospun, obtains Co2+Salt/PVP composite cellulosic membranes, spinning voltage 21kV；Spacing 13cm of the shower nozzle to receiver board；Ambient humidity
60%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and are made
Its pre-oxidation and carbonization, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 4.5 DEG C/min；Calcining heat is 400 DEG C；Calcination time is 4h；Calcining
Atmosphere is air；
The parameter of carbonization is：Heating rate is 6 DEG C/min；Calcining heat is 900 DEG C；Calcination time is 4h；Calcination atmosphere
It is air.
The present embodiment Co3O4Carbon nano-fiber is in 100mAg-1Current density under cycle performance and embodiment 1 it is close,
Show Co3O4Carbon nano-fiber negative material has preferable capability retention and preferable stable circulation under high current density
Property, being applied to sodium-ion battery negative pole has excellent charge-discharge magnification performance.
Embodiment 6, sodium-ion battery Co3O4The method for manufacturing electric spinning of carbon nano-fiber, comprises the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 it is mixed
In conjunction solution, Co2+The quality of salt is 0.29g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then again
Polyvinylpyrrolidone (PVP) powder is added to mixed solution, stirring obtains uniform Electrospun precursor liquid, polyvinyl pyrrole
Alkanone (PVP) is 0.15g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is cobalt nitrate；
Described organic solvent is N,N-dimethylformamide (DMF)；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carry out it is quiet
Electrospun, obtains Co2+Salt/PVP composite cellulosic membranes, spinning voltage 23kV；Spacing 18cm of the shower nozzle to receiver board；Ambient humidity
50%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and are made
Its pre-oxidation and carbonization, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 6 DEG C/min；Calcining heat is 370 DEG C；Calcination time is 4.5h；Calcining
Atmosphere is air；
The parameter of carbonization is：Heating rate is 8 DEG C/min；Calcining heat is 850 DEG C；Calcination time is 4.5h；Calcining gas
Atmosphere is air.
The present embodiment Co3O4Carbon nano-fiber is in 100mAg-1Current density under cycle performance and embodiment 1 it is close,
Show Co3O4Carbon nano-fiber negative material has preferable capability retention and preferable stable circulation under high current density
Property, being applied to sodium-ion battery negative pole has excellent charge-discharge magnification performance.
Claims (8)
1. sodium-ion battery Co3O4The method for manufacturing electric spinning of carbon nano-fiber, it is characterised in that comprise the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 mixing is molten
In liquid, Co2+The quality of salt is 0.14~0.29g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then
Polyvinylpyrrolidone (PVP) powder is added to mixed solution again, stirring obtains uniform Electrospun precursor liquid, polyethylene pyrrole
Pyrrolidone (PVP) is 0.08~0.15g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is selected from any one in cobalt chloride, cobalt nitrate or cobaltous sulfate；
Described organic solvent is selected from any one in ethanol, methyl alcohol or N,N-dimethylformamide (DMF)；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carries out Static Spinning
Silk, obtains Co2+Salt/PVP composite cellulosic membranes, 12~25kV of spinning voltage；Spacing 8~20cm of the shower nozzle to receiver board；Environmental wet
Degree 30~60%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and make its pre- oxygen
Change and be carbonized, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 0.5~6 DEG C/min；Calcining heat is 300~400 DEG C；Calcination time be 2~
5h；Calcination atmosphere is air；
The parameter of carbonization is：Heating rate is 3~8 DEG C/min；Calcining heat is 700~900 DEG C；Calcination time is 2~5h；Forge
Burning atmosphere is air.
2. the Co that prepared by method according to claim 13O4Carbon nano-fiber, it is characterised in that：Its Co3O4Nanocrystal
Pattern is ultra-thin hexagonal nano sheet, and particle diameter is 5~20nm, is equably embedded in the diameter about carbon nano-fiber of 150nm.
3. sodium-ion battery Co according to claim 13O4The method for manufacturing electric spinning of carbon nano-fiber, its feature exists
In comprising the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 mixing is molten
In liquid, Co2+The quality of salt is 0.14g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then again to mixed
Close solution and add polyvinylpyrrolidone (PVP) powder, stirring obtains uniform Electrospun precursor liquid, polyvinylpyrrolidone
(PVP) it is 0.08g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is cobalt nitrate；
Described organic solvent is ethanol；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carries out Static Spinning
Silk, obtains Co2+Salt/PVP composite cellulosic membranes, spinning voltage 15kV；Spacing 12cm of the shower nozzle to receiver board；Ambient humidity 50%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and make its pre- oxygen
Change and be carbonized, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 2 DEG C/min；Calcining heat is 350 DEG C；Calcination time is 2h；Calcination atmosphere is
Air；
The parameter of carbonization is：Heating rate is 4 DEG C/min；Calcining heat is 800 DEG C；Calcination time is 2h；Calcination atmosphere is sky
Gas.
4. sodium-ion battery Co according to claim 13O4The method for manufacturing electric spinning of carbon nano-fiber, its feature exists
In comprising the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 mixing is molten
In liquid, Co2+The quality of salt is 0.16g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then again to mixed
Close solution and add polyvinylpyrrolidone (PVP) powder, stirring obtains uniform Electrospun precursor liquid, polyvinylpyrrolidone
(PVP) it is 0.10g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is cobalt chloride；
Described organic solvent is methyl alcohol；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carries out Static Spinning
Silk, obtains Co2+Salt/PVP composite cellulosic membranes, spinning voltage 12kV；Spacing 8cm of the shower nozzle to receiver board；Ambient humidity 35%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and make its pre- oxygen
Change and be carbonized, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 1 DEG C/min；Calcining heat is 300 DEG C；Calcination time is 2.5h；Calcination atmosphere
It is air；
The parameter of carbonization is：Heating rate is 4 DEG C/min；Calcining heat is 700 DEG C；Calcination time is 2.5h；Calcination atmosphere is
Air.
5. sodium-ion battery Co according to claim 13O4The method for manufacturing electric spinning of carbon nano-fiber, its feature exists
In comprising the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 mixing is molten
In liquid, Co2+The quality of salt is 0.18g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then again to mixed
Close solution and add polyvinylpyrrolidone (PVP) powder, stirring obtains uniform Electrospun precursor liquid, polyvinylpyrrolidone
(PVP) it is 0.12g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is cobaltous sulfate；
Described organic solvent is N,N-dimethylformamide (DMF)；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carries out Static Spinning
Silk, obtains Co2+Salt/PVP composite cellulosic membranes, spinning voltage 18kV；Spacing 10cm of the shower nozzle to receiver board；Ambient humidity 30%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and make its pre- oxygen
Change and be carbonized, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 0.5 DEG C/min；Calcining heat is 320 DEG C；Calcination time is 3h；Calcination atmosphere
It is air；
The parameter of carbonization is：Heating rate is 3 DEG C/min；Calcining heat is 750 DEG C；Calcination time is 3h；Calcination atmosphere is sky
Gas.
6. sodium-ion battery Co according to claim 13O4The method for manufacturing electric spinning of carbon nano-fiber, its feature exists
In comprising the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 mixing is molten
In liquid, Co2+The quality of salt is 0.20g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then again to mixed
Close solution and add polyvinylpyrrolidone (PVP) powder, stirring obtains uniform Electrospun precursor liquid, polyvinylpyrrolidone
(PVP) it is 0.13g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is cobalt chloride；
Described organic solvent is ethanol；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carries out Static Spinning
Silk, obtains Co2+Salt/PVP composite cellulosic membranes, spinning voltage 25kV；Spacing 20cm of the shower nozzle to receiver board；Ambient humidity 40%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and make its pre- oxygen
Change and be carbonized, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 3 DEG C/min；Calcining heat is 360 DEG C；Calcination time is 5h；Calcination atmosphere is
Air；
The parameter of carbonization is：Heating rate is 5 DEG C/min；Calcining heat is 800 DEG C；Calcination time is 5h；Calcination atmosphere is sky
Gas.
7. sodium-ion battery Co according to claim 13O4The method for manufacturing electric spinning of carbon nano-fiber, its feature exists
In comprising the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 mixing is molten
In liquid, Co2+The quality of salt is 0.26g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then again to mixed
Close solution and add polyvinylpyrrolidone (PVP) powder, stirring obtains uniform Electrospun precursor liquid, polyvinylpyrrolidone
(PVP) it is 0.13g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is cobaltous sulfate；
Described organic solvent is methyl alcohol；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carries out Static Spinning
Silk, obtains Co2+Salt/PVP composite cellulosic membranes, spinning voltage 21kV；Spacing 13cm of the shower nozzle to receiver board；Ambient humidity 60%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and make its pre- oxygen
Change and be carbonized, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 4.5 DEG C/min；Calcining heat is 400 DEG C；Calcination time is 4h；Calcination atmosphere
It is air；
The parameter of carbonization is：Heating rate is 6 DEG C/min；Calcining heat is 900 DEG C；Calcination time is 4h；Calcination atmosphere is sky
Gas.
8. sodium-ion battery Co according to claim 13O4The method for manufacturing electric spinning of carbon nano-fiber, its feature exists
In comprising the following steps：
1) configuration of Electrospun precursor liquid：By Co2+Salt is dissolved in deionized water and organic solvent according to volume ratio 1:1 mixing is molten
In liquid, Co2+The quality of salt is 0.29g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；Then again to mixed
Close solution and add polyvinylpyrrolidone (PVP) powder, stirring obtains uniform Electrospun precursor liquid, polyvinylpyrrolidone
(PVP) it is 0.15g/mL with the mass volume ratio of deionized water and organic solvent mixed solution；
Described Co2+Salt is cobalt nitrate；
Described organic solvent is N,N-dimethylformamide (DMF)；
Described polyvinylpyrrolidone (PVP) molecular weight is 1,300,000；
2) electrical spinning method prepares Co2+Salt/PVP composite cellulosic membranes：With step 1) the Electrospun precursor liquid that obtains carries out Static Spinning
Silk, obtains Co2+Salt/PVP composite cellulosic membranes, spinning voltage 23kV；Spacing 18cm of the shower nozzle to receiver board；Ambient humidity 50%；
3)Co3O4The preparation of carbon nano-fiber：By step 2) Co that obtains2+Salt/PVP composite cellulosic membranes are calcined, and make its pre- oxygen
Change and be carbonized, obtain Co3O4Carbon nano-fiber,
The parameter of pre-oxidation is：Heating rate is 6 DEG C/min；Calcining heat is 370 DEG C；Calcination time is 4.5h；Calcination atmosphere
It is air；
The parameter of carbonization is：Heating rate is 8 DEG C/min；Calcining heat is 850 DEG C；Calcination time is 4.5h；Calcination atmosphere is
Air.
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| CN107237008A (en) * | 2017-06-01 | 2017-10-10 | 赵云飞 | Preparation method, electrode and the electrochemical sensor of porous nano-fibre |
| CN107579238A (en) * | 2017-09-13 | 2018-01-12 | 电子科技大学 | Cobaltosic oxide FTO nano wires lithium cell cathode material and preparation method |
| CN107723849A (en) * | 2017-10-31 | 2018-02-23 | 西北工业大学 | A kind of preparation method of high-ratio surface hybridizing carbon nano fibers |
| CN108642606A (en) * | 2018-04-11 | 2018-10-12 | 西安交通大学 | Cobaltosic oxide/carbon nano-fiber composite material and its preparation method and application |
| CN109755033A (en) * | 2019-03-08 | 2019-05-14 | 桂林电子科技大学 | A kind of carbon fiber loaded cobalt/cobalt oxide composite material and preparation method and application |
| CN110459740A (en) * | 2019-07-16 | 2019-11-15 | 五邑大学 | A kind of carbon nanotube cladding cobalt oxide material and its preparation method and application |
| CN111525117A (en) * | 2020-05-11 | 2020-08-11 | 喻明兵 | Three-dimensional porous carbon coated Co3O4The negative electrode material of the sodium ion battery and the preparation method thereof |
| CN111554892A (en) * | 2020-04-24 | 2020-08-18 | 宁波大学 | Lithium battery negative electrode material Co3O4Preparation method of nano-fiber |
| CN112251847A (en) * | 2020-10-15 | 2021-01-22 | 广东工业大学 | Preparation method and application of molybdenum phosphide/carbon fiber composite material |
| CN115893510A (en) * | 2022-11-24 | 2023-04-04 | 贝特瑞(四川)新材料科技有限公司 | Anode material for nitrogen-doped honeycomb type sodium ion battery and preparation method thereof |
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| CN107237008A (en) * | 2017-06-01 | 2017-10-10 | 赵云飞 | Preparation method, electrode and the electrochemical sensor of porous nano-fibre |
| CN107579238A (en) * | 2017-09-13 | 2018-01-12 | 电子科技大学 | Cobaltosic oxide FTO nano wires lithium cell cathode material and preparation method |
| CN107579238B (en) * | 2017-09-13 | 2019-11-01 | 电子科技大学 | Cobaltosic oxide-FTO nano wire lithium cell cathode material and preparation method |
| CN107723849A (en) * | 2017-10-31 | 2018-02-23 | 西北工业大学 | A kind of preparation method of high-ratio surface hybridizing carbon nano fibers |
| CN108642606A (en) * | 2018-04-11 | 2018-10-12 | 西安交通大学 | Cobaltosic oxide/carbon nano-fiber composite material and its preparation method and application |
| CN109755033A (en) * | 2019-03-08 | 2019-05-14 | 桂林电子科技大学 | A kind of carbon fiber loaded cobalt/cobalt oxide composite material and preparation method and application |
| CN110459740A (en) * | 2019-07-16 | 2019-11-15 | 五邑大学 | A kind of carbon nanotube cladding cobalt oxide material and its preparation method and application |
| CN110459740B (en) * | 2019-07-16 | 2022-06-24 | 五邑大学 | Carbon nanotube coated cobalt oxide material and preparation method and application thereof |
| CN111554892A (en) * | 2020-04-24 | 2020-08-18 | 宁波大学 | Lithium battery negative electrode material Co3O4Preparation method of nano-fiber |
| CN111554892B (en) * | 2020-04-24 | 2021-07-30 | 宁波大学 | Lithium battery negative electrode material Co3O4Preparation method of nano-fiber |
| CN111525117A (en) * | 2020-05-11 | 2020-08-11 | 喻明兵 | Three-dimensional porous carbon coated Co3O4The negative electrode material of the sodium ion battery and the preparation method thereof |
| CN111525117B (en) * | 2020-05-11 | 2021-10-22 | 江苏圳威新材料有限公司 | Three-dimensional porous carbon coated Co3O4The negative electrode material of the sodium ion battery and the preparation method thereof |
| CN112251847A (en) * | 2020-10-15 | 2021-01-22 | 广东工业大学 | Preparation method and application of molybdenum phosphide/carbon fiber composite material |
| CN115893510A (en) * | 2022-11-24 | 2023-04-04 | 贝特瑞(四川)新材料科技有限公司 | Anode material for nitrogen-doped honeycomb type sodium ion battery and preparation method thereof |
| CN115893510B (en) * | 2022-11-24 | 2024-03-12 | 贝特瑞(四川)新材料科技有限公司 | Negative electrode material for nitrogen-doped honeycomb type sodium ion battery and preparation method thereof |
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