CN109360739A - Load the preparation method of the carbon nanofiber electrode material of nickel nickel - Google Patents
Load the preparation method of the carbon nanofiber electrode material of nickel nickel Download PDFInfo
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- CN109360739A CN109360739A CN201811543568.2A CN201811543568A CN109360739A CN 109360739 A CN109360739 A CN 109360739A CN 201811543568 A CN201811543568 A CN 201811543568A CN 109360739 A CN109360739 A CN 109360739A
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- nickel
- wood fibre
- electrode material
- nanometer wood
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- 239000007772 electrode material Substances 0.000 title claims abstract description 81
- 239000002134 carbon nanofiber Substances 0.000 title claims abstract description 68
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- XIKYYQJBTPYKSG-UHFFFAOYSA-N nickel Chemical compound [Ni].[Ni] XIKYYQJBTPYKSG-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229920002522 Wood fibre Polymers 0.000 claims abstract description 85
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000000463 material Substances 0.000 claims abstract description 39
- VMWYVTOHEQQZHQ-UHFFFAOYSA-N methylidynenickel Chemical compound [Ni]#[C] VMWYVTOHEQQZHQ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 150000002815 nickel Chemical class 0.000 claims abstract description 27
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 24
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 18
- 239000012498 ultrapure water Substances 0.000 claims abstract description 18
- 238000011068 loading method Methods 0.000 claims abstract description 14
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 13
- 239000012266 salt solution Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 88
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000012545 processing Methods 0.000 claims description 23
- 238000005255 carburizing Methods 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 230000035945 sensitivity Effects 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 239000003792 electrolyte Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 238000000265 homogenisation Methods 0.000 claims description 12
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 claims description 11
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 claims description 4
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims description 4
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 239000002070 nanowire Substances 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 229910000480 nickel oxide Inorganic materials 0.000 abstract description 22
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 17
- 229910052799 carbon Inorganic materials 0.000 description 13
- 210000004027 cell Anatomy 0.000 description 11
- 235000019441 ethanol Nutrition 0.000 description 11
- 238000004146 energy storage Methods 0.000 description 9
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 7
- 238000003763 carbonization Methods 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000006258 conductive agent Substances 0.000 description 4
- 229910001453 nickel ion Inorganic materials 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000011267 electrode slurry Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 210000004508 polar body Anatomy 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/626—Metals
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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Abstract
The invention discloses a kind of preparation methods of carbon nanofiber electrode material for loading nickel nickel, comprising the following steps: (1) disperses nanometer wood fibre in ultrapure water, nanometer wood fibre film is dried to obtain after vacuum filtration;(2) nanometer wood fibre film obtained in step (1) is placed in nickel salt solution after impregnating and takes out drying, then high temperature cabonization handles to obtain nickel carbon nano-fiber film material;(3) nickel carbon nano-fiber film material obtained in step (2) is handled by electroxidation and obtains nickel-loaded/nickel oxide carbon nanofiber electrode material.The present invention combines nickel oxide with carbon nano-fiber, in conjunction with the excellent properties of the two, compensates for the use limitation of unitary electrode material, considerably increases the chemical property of electrode material.
Description
Technical field
The invention belongs to energy storage material field more particularly to a kind of preparation methods of electrode.
Background technique
Energy storage device is a kind of device that energy conversion and storage may be implemented.With the continuous development of modernization,
The demand of energy storage device is also being continuously increased, therefore, urgent need develops high performance energy storage device.Energy storage device usually divides
For battery and capacitor two major classes, battery energy density is big and power density is small, and capacitor is then opposite.Above-mentioned difference mainly depends on
It is closely related with electrode material in the energy storage mechnism of energy storage device.
Electrode material is the important component of energy storage device, and common electrode material is mainly transition metal oxide,
Such as nickel oxide, ruthenium-oxide, cobalt oxide and carbon material, such as graphene, carbon nanotube, activated carbon.Wherein metal oxide
Theoretical capacity with higher, but the problems such as poorly conductive, specific surface area are smaller, voltage range is relatively narrow, limits metal oxidation
Further development of the object in energy storage material.Carbon material is with good electric conductivity and has wider voltage window, but theoretical
Capacity is lower, contact resistance is larger.
The drawbacks of in order to solve above-mentioned material, can be used compound mode and combine metal oxide with same with carbon material
When obtain both advantage.But the existing method for preparing electrode frequently be by active material and binder, conductive agent
It is coated with etc. being mixed after slurry on collector, wherein the addition of binder and conductive agent largely influences electrode
The resistance and wetability of material, to influence its electric conductivity and capacitive property.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, one kind is provided
The preparation method of carbon nanofiber electrode material with superior electrical conductivity and capacitive load nickel nickel.On solving
State technical problem, technical solution proposed by the present invention are as follows:
A kind of preparation method for the carbon nanofiber electrode material loading nickel nickel, comprising the following steps:
(1) it disperses nanometer wood fibre in ultrapure water, nanometer wood fibre film is dried to obtain after vacuum filtration;It receives
Rice wood fibre has good film forming, dry because drainage weightlessness makes its fiber self assembly form a film during suction filtration
After can obtain film flexible;
(2) nanometer wood fibre film obtained in step (1) is placed in nickel salt solution after impregnating and takes out drying, then is high
Warm carbonization treatment obtains nickel carbon nano-fiber film material;When high temperature cabonization, nickel ion can be reduced into nickel simple substance;
(3) by nickel carbon nano-fiber film material obtained in step (2) by electroxidation handle i.e. obtain nickel-loaded/
The carbon nanofiber electrode material of nickel oxide;The effect of electroxidation processing is that elemental nickel is oxidized to nickel oxide, increases material
Capacitive property.
In above-mentioned preparation method, needs that nanometer wood fibre is first prepared into form of film and is soaked in nickel salt solution again,
If nanometer wood fibre first impregnates absorption nickel ion, it is difficult to make nickel ion be attached to nanometer wood fibre in the form of filtering
It goes up and forms a film, because nickel ion is dissolved in water, be easy to take away with water during suction filtration, even if there are part of nickel ionic adsorption, point
Cloth also can be uneven.Absorption can solve the problems such as absorption is uneven, load capacity is not high, while side after experimental study shows film forming
Method is simple and easy.
In above-mentioned preparation method, it is preferred that the nanometer wood fibre passes through sour water solution-high pressure homogenization method by cellulose powder
It is prepared;Nickel salt in the nickel salt solution is at least one of six water nickel chlorides, nickel sulfate hexahydrate or six water nickel nitrates.
In above-mentioned preparation method, it is preferred that control is carried on nanometer wood fibre film when impregnating in the step (2)
The quality of nickel salt account for the 10%-70% of nickel carbon nano-fiber film material gross mass, it is furthermore preferred that being 30-60%.Nickel salt
Load capacity have a large effect to the performance of subsequent electrode material, the load capacity of nickel salt needs to control preferred control and is
The chemical property of 30-60%, electrode material are optimal.
In above-mentioned preparation method, it is preferred that control nanometer wood fibre when dispersing nanometer wood fibre in ultrapure water
The mass concentration of solution is 0.5-0.8wt.%.The mass concentration of nanometer wood fibre has the porosity of the film of formation biggish
It influences, the control of above-mentioned mass concentration and the control of high temperature cabonization cooperate, the available optimal electrode material of chemical property
Material.
In above-mentioned preparation method, it is preferred that the high temperature cabonization processing carries out in tube furnace, under nitrogen protection, and
Keeping carburizing temperature is 450-1000 DEG C, and heating rate is 5-10 DEG C/min, soaking time 1-3h.The technique of carbonization treatment is joined
The hole result tool of several pairs of electrode materials has a certain impact, and the determination of above-mentioned high temperature cabonization temperature is conducive to obtain electrochemistry
The excellent electrode material of energy.
In above-mentioned preparation method, it is preferred that the electroxidation processing is electric for nickel carbon nano-fiber film material is placed in three
It in polar body system, then is handled using potentiostatic method, the potassium hydroxide solution (1mol/L or 6mol/L) that electrolyte uses when processing,
Control voltage is 0.8-1.2V, and sensitivity (sensitivity) is set as 1.0e-1, the processing time is 30-600s (preferred
For 300-600s).The control of the technological parameter of above-mentioned electroxidation processing is very big on electrode performance influence, electroxidation processing parameter
Control can control the mass ratio of elemental nickel, nickel oxide and nanometer wood fibre, to regulate and control to obtain optimal electrochemistry
Energy.
Nickel, nickel oxide can be uniformly carried on carbon nano-fiber by the electrode material that the present invention is prepared, carbon nanometer
Fiber itself has certain intensity and electric conductivity, can provide while improving the electric conductivity of electrode material for nickel oxide
The forming process of skeleton and support system, oxide is not easy to reunite, can form nanostructure, so that the thin-film electrode material
The advantages of being compounded with nickel oxide and carbon.In addition, the electrode material is the form of film, it can use, can save directly as electrode
Go the links such as milling slurrying.
The present invention prepares dense by the mass ratio of combined regulating nanometer wood fibre and nickel salt, nanometer wood fibre when electrode
Spending (water content) and electroxidation treatment process etc. can be to regulate and control pattern and the performance of electrode material to obtain optimal electricity
Chemical result.
The electrode that the present invention is prepared can be used as battery, such as the electrode material of lithium ion battery, nickel-zinc cell, can also
For use as capacitor, such as the electrode material of Asymmetric Supercapacitor.
Compared with the prior art, the advantages of the present invention are as follows:
1, the present invention combines nickel oxide with carbon nano-fiber, in conjunction with the excellent properties of the two, compensates for unitary electrode
The use of material limits, and considerably increases the chemical property of electrode material.
2, the present invention is when preparing electrode material, without preparing electrode slurry, reduces the use of binder, conductive agent,
The resistance and wetability that influence electrode material is added for avoiding binder, conductive agent, have the electrode material in the present invention
For excellent electric conductivity and capacitive character.
3, electrode material of the invention is form of film, can be used directly as electrode.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is the flow diagram of preparation method in the embodiment of the present invention.
Fig. 2 is that (a is nanometer wood fibre film in figure for the macrograph of the electrode material being prepared in embodiment 1;B is
Nickel carbon nano-fiber film material).
Fig. 3 is the SEM figure for the electrode material being prepared in embodiment 1.
Fig. 4 is the AC impedance figure for the electrode material being prepared in embodiment 1.
Specific embodiment
To facilitate the understanding of the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1:
As shown in Figure 1, a kind of preparation method for the carbon nanofiber electrode material for loading nickel nickel, including following step
It is rapid:
(1) it disperses 50g nanometer wood fibre (being prepared by cellulose powder by sour water solution-high pressure homogenization method) in super
In pure water (mass concentration of control nanometer wood fibre is 0.5wt.%), spontaneously dried after vacuum filtration, floatation of filter film obtains
Transparent nanometer wood fibre film;
(2) after nanometer wood fibre film obtained in step (1) being impregnated in the nickel sulfate hexahydrate solution of 1mol/L
Take out spontaneously dry, control nickel salt load capacity for nanometer wood fibre total film mass (including nickel salt and nanometer wood fibre it is thin
The quality of film, similarly hereinafter) 60%.Nickel carbon nano-fiber film material is obtained then at tube furnace high temperature carbonization treatment;Wherein,
Controlling carburizing temperature is 700 DEG C, and heating rate is 5 DEG C/min, keeps the temperature 2h, and be passed through nitrogen protection;
(3) nickel carbon nano-fiber film material obtained in step (2) is placed in three electrode electrolysers and carries out constant potential
Method processing, then nickel-loaded/nickel oxide carbon nanofiber electrode material is obtained after being cleaned with ethyl alcohol and ultrapure water;Wherein,
Electrolyte in electrolytic cell uses the potassium hydroxide of 6mol/L, and control voltage is 1V, and sensitivity is set as 1.0e-1, handle the time
For 600s.
The macrograph for the electrode material being prepared in the present embodiment is as shown in Fig. 2, nanometer wood fibre is thin as seen from the figure
Membranaceous structure still can be kept after film absorption nickel salt and carbonization.The SEM for the electrode material being prepared in the present embodiment schemes
As shown in figure 3, as seen from the figure, nano-nickel oxide is evenly affixed to carbon nano-fiber surface.Electrification is carried out to above-mentioned electrode material
Performance test is learned, it is 2.5 Ω that as shown in Figure 4, the resistance value of the electrode material is lower for AC impedance, and conductivity is good.The present embodiment
In electrode material chemical property it is preferable, the specific capacitance of prepared electrode material is 116F/g.
Embodiment 2:
As shown in Figure 1, a kind of preparation method for the carbon nanofiber electrode material for loading nickel nickel, including following step
It is rapid:
(1) it disperses 50g nanometer wood fibre (being prepared by cellulose powder by sour water solution-high pressure homogenization method) in super
In pure water (mass concentration of control nanometer wood fibre is 0.5wt.%), spontaneously dried after vacuum filtration, floatation of filter film obtains
Transparent nanometer wood fibre film;
(2) after nanometer wood fibre film obtained in step (1) being impregnated in the nickel sulfate hexahydrate solution of 1mol/L
It takes out and spontaneously dries, control nickel salt load capacity is the 60% of nanometer wood fibre total film mass.Then at tube furnace high temperature carbon
Change handles to obtain nickel carbon nano-fiber film material;Wherein, control carburizing temperature is 800 DEG C, and heating rate is 5 DEG C/min, is protected
Warm 2h, and it is passed through nitrogen protection;
(3) nickel carbon nano-fiber film material obtained in step (2) is placed in three electrode electrolysers and carries out constant potential
Method processing, then nickel-loaded/nickel oxide carbon nanofiber electrode material is obtained after being cleaned with ethyl alcohol and ultrapure water;Wherein,
Electrolyte in electrolytic cell uses the potassium hydroxide of 6mol/L, and control voltage is 1V, and sensitivity is set as 1.0e-1, handle the time
For 100s.
The resistance value of the electrode material of the electrode material prepared in the present embodiment is lower, is 1 Ω, specific capacitance 80F/
g。
Embodiment 3:
As shown in Figure 1, a kind of preparation method for the carbon nanofiber electrode material for loading nickel nickel, including following step
It is rapid:
(1) it disperses 50g nanometer wood fibre (being prepared by cellulose powder by sour water solution-high pressure homogenization method) in super
In pure water (mass concentration of control nanometer wood fibre is 0.5wt.%), spontaneously dried after vacuum filtration, floatation of filter film obtains
Transparent nanometer wood fibre film;
(2) after nanometer wood fibre film obtained in step (1) being impregnated in the six water nickel chloride solutions of 1mol/L
It takes out and spontaneously dries, control nickel salt load capacity is the 10% of nanometer wood fibre total film mass.Then at tube furnace high temperature carbon
Change handles to obtain nickel carbon nano-fiber film material;Wherein, control carburizing temperature is 800 DEG C, and heating rate is 5 DEG C/min, is protected
Warm 2h, and it is passed through nitrogen protection;
(3) nickel carbon nano-fiber film material obtained in step (2) is placed in three electrode electrolysers and carries out constant potential
Method processing, then nickel-loaded/nickel oxide carbon nanofiber electrode material is obtained after being cleaned with ethyl alcohol and ultrapure water;Wherein,
Electrolyte in electrolytic cell uses the potassium hydroxide of 6mol/L, and control voltage is 1V, and sensitivity is set as 1.0e-1, handle the time
For 400s.
The resistance value of the electrode material of the electrode material prepared in the present embodiment is lower, is 1.5 Ω, and specific capacitance is
40F/g。
Embodiment 4:
As shown in Figure 1, a kind of preparation method for the carbon nanofiber electrode material for loading nickel nickel, including following step
It is rapid:
(1) it disperses 50g nanometer wood fibre (being prepared by cellulose powder by sour water solution-high pressure homogenization method) in super
In pure water (mass concentration of control nanometer wood fibre is 0.5wt.%), spontaneously dried after vacuum filtration, floatation of filter film obtains
Transparent nanometer wood fibre film;
(2) after nanometer wood fibre film obtained in step (1) being impregnated in the six water nickel chloride solutions of 5mol/L
It takes out and spontaneously dries, control nickel salt load capacity is the 30% of nanometer wood fibre total film mass.Then at tube furnace high temperature carbon
Change handles to obtain nickel carbon nano-fiber film material;Wherein, control carburizing temperature is 1000 DEG C, and heating rate is 5 DEG C/min,
2h is kept the temperature, and is passed through nitrogen protection;
(3) nickel carbon nano-fiber film material obtained in step (2) is placed in three electrode electrolysers and carries out constant potential
Method processing, then nickel-loaded/nickel oxide carbon nanofiber electrode material is obtained after being cleaned with ethyl alcohol and ultrapure water;Wherein,
Electrolyte in electrolytic cell uses the potassium hydroxide of 6mol/L, and control voltage is 1V, and sensitivity is set as 1.0e-1, handle the time
For 100s.
The resistance value of the electrode material of the electrode material prepared in the present embodiment is lower, is 1 Ω, specific capacitance 20F/
g。
Embodiment 5:
As shown in Figure 1, a kind of preparation method for the carbon nanofiber electrode material for loading nickel nickel, including following step
It is rapid:
(1) it disperses 50g nanometer wood fibre (being prepared by cellulose powder by sour water solution-high pressure homogenization method) in super
In pure water (mass concentration of control nanometer wood fibre is 0.5wt.%), spontaneously dried after vacuum filtration, floatation of filter film obtains
Transparent nanometer wood fibre film;
(2) after nanometer wood fibre film obtained in step (1) being impregnated in the six water nickel chloride solutions of 5mol/L
It takes out and spontaneously dries, control nickel salt load capacity is the 48% of nanometer wood fibre total film mass.Then at tube furnace high temperature carbon
Change handles to obtain nickel carbon nano-fiber film material;Wherein, control carburizing temperature is 700 DEG C, and heating rate is 5 DEG C/min, is protected
Warm 2h, and it is passed through nitrogen protection;
(3) nickel carbon nano-fiber film material obtained in step (2) is placed in three electrode electrolysers and carries out constant potential
Method processing, then nickel-loaded/nickel oxide carbon nanofiber electrode material is obtained after being cleaned with ethyl alcohol and ultrapure water;Wherein,
Electrolyte in electrolytic cell uses the potassium hydroxide of 6mol/L, and control voltage is 1V, and sensitivity is set as 1.0e-1, handle the time
For 450s.
The resistance value of the electrode material of the electrode material prepared in the present embodiment is lower, is 0.9 Ω, and specific capacitance is
125F/g。
Embodiment 6:
As shown in Figure 1, a kind of preparation method for the carbon nanofiber electrode material for loading nickel nickel, including following step
It is rapid:
(1) it disperses 50g nanometer wood fibre (being prepared by cellulose powder by sour water solution-high pressure homogenization method) in super
In pure water (mass concentration of control nanometer wood fibre is 0.5wt.%), spontaneously dried after vacuum filtration, floatation of filter film obtains
Transparent nanometer wood fibre film;
(2) after nanometer wood fibre film obtained in step (1) being impregnated in the six water nickel chloride solutions of 5mol/L
It takes out and spontaneously dries, control nickel salt load capacity is the 55% of nanometer wood fibre total film mass.Then at tube furnace high temperature carbon
Change handles to obtain nickel carbon nano-fiber film material;Wherein, control carburizing temperature is 700 DEG C, and heating rate is 5 DEG C/min, is protected
Warm 2h, and it is passed through nitrogen protection;
(3) nickel carbon nano-fiber film material obtained in step (2) is placed in three electrode electrolysers and carries out constant potential
Method processing, then nickel-loaded/nickel oxide carbon nanofiber electrode material is obtained after being cleaned with ethyl alcohol and ultrapure water;Wherein,
Electrolyte in electrolytic cell uses the potassium hydroxide of 6mol/L, and control voltage is 1V, and sensitivity is set as 1.0e-1, handle the time
For 450s.
The resistance value of the electrode material of the electrode material prepared in the present embodiment is lower, is 1 Ω, and specific capacitance is
112F/g。
Embodiment 7:
As shown in Figure 1, a kind of preparation method for the carbon nanofiber electrode material for loading nickel nickel, including following step
It is rapid:
(1) it disperses 50g nanometer wood fibre (being prepared by cellulose powder by sour water solution-high pressure homogenization method) in super
In pure water (mass concentration of control nanometer wood fibre is 0.5wt.%), spontaneously dried after vacuum filtration, floatation of filter film obtains
Transparent nanometer wood fibre film;
(2) after nanometer wood fibre film obtained in step (1) being impregnated in the six water nickel chloride solutions of 5mol/L
It takes out and spontaneously dries, control nickel salt load capacity is the 40% of nanometer wood fibre total film mass.Then at tube furnace high temperature carbon
Change handles to obtain nickel carbon nano-fiber film material;Wherein, control carburizing temperature is 700 DEG C, and heating rate is 5 DEG C/min, is protected
Warm 2h, and it is passed through nitrogen protection;
(3) nickel carbon nano-fiber film material obtained in step (2) is placed in three electrode electrolysers and carries out constant potential
Method processing, then nickel-loaded/nickel oxide carbon nanofiber electrode material is obtained after being cleaned with ethyl alcohol and ultrapure water;Wherein,
Electrolyte in electrolytic cell uses the potassium hydroxide of 6mol/L, and control voltage is 1V, and sensitivity is set as 1.0e-1, handle the time
For 450s.
The resistance value of the electrode material of the electrode material prepared in the present embodiment is lower, is 1 Ω, and specific capacitance is
100F/g。
Embodiment 8:
As shown in Figure 1, a kind of preparation method for the carbon nanofiber electrode material for loading nickel nickel, including following step
It is rapid:
(1) it disperses 50g nanometer wood fibre (being prepared by cellulose powder by sour water solution-high pressure homogenization method) in super
In pure water (mass concentration of control nanometer wood fibre is 0.5wt.%), spontaneously dried after vacuum filtration, floatation of filter film obtains
Transparent nanometer wood fibre film;
(2) after nanometer wood fibre film obtained in step (1) being impregnated in the six water nickel chloride solutions of 5mol/L
It takes out and spontaneously dries, control nickel salt load capacity is the 48% of nanometer wood fibre total film mass.Then at tube furnace high temperature carbon
Change handles to obtain nickel carbon nano-fiber film material;Wherein, control carburizing temperature is 700 DEG C, and heating rate is 5 DEG C/min, is protected
Warm 2h, and it is passed through nitrogen protection;
(3) nickel carbon nano-fiber film material obtained in step (2) is placed in three electrode electrolysers and carries out constant potential
Method processing, then nickel-loaded/nickel oxide carbon nanofiber electrode material is obtained after being cleaned with ethyl alcohol and ultrapure water;Wherein,
Electrolyte in electrolytic cell uses the potassium hydroxide of 6mol/L, and control voltage is 1V, and sensitivity is set as 1.0e-1, handle the time
For 550s.
The resistance value of the electrode material of the electrode material prepared in the present embodiment is lower, is 1.1 Ω, and specific capacitance is
120F/g。
Embodiment 9:
As shown in Figure 1, a kind of preparation method for the carbon nanofiber electrode material for loading nickel nickel, including following step
It is rapid:
(1) it disperses 50g nanometer wood fibre (being prepared by cellulose powder by sour water solution-high pressure homogenization method) in super
In pure water (mass concentration of control nanometer wood fibre is 0.8wt.%), spontaneously dried after vacuum filtration, floatation of filter film obtains
Transparent nanometer wood fibre film;
(2) after nanometer wood fibre film obtained in step (1) being impregnated in the six water nickel chloride solutions of 5mol/L
It takes out and spontaneously dries, control nickel salt load capacity is the 48% of nanometer wood fibre total film mass.Then at tube furnace high temperature carbon
Change handles to obtain nickel carbon nano-fiber film material;Wherein, control carburizing temperature is 1000 DEG C, and heating rate is 5 DEG C/min,
2h is kept the temperature, and is passed through nitrogen protection;
(3) nickel carbon nano-fiber film material obtained in step (2) is placed in three electrode electrolysers and carries out constant potential
Method processing, then nickel-loaded/nickel oxide carbon nanofiber electrode material is obtained after being cleaned with ethyl alcohol and ultrapure water;Wherein,
Electrolyte in electrolytic cell uses the potassium hydroxide of 6mol/L, and control voltage is 1V, and sensitivity is set as 1.0e-1, handle the time
For 350s.
The resistance value of the electrode material of the electrode material prepared in the present embodiment is lower, is 1 Ω, and specific capacitance is
110F/g。
Embodiment 10:
As shown in Figure 1, a kind of preparation method for the carbon nanofiber electrode material for loading nickel nickel, including following step
It is rapid:
(1) it disperses 50g nanometer wood fibre (being prepared by cellulose powder by sour water solution-high pressure homogenization method) in super
In pure water (mass concentration of control nanometer wood fibre is 0.5wt.%), spontaneously dried after vacuum filtration, floatation of filter film obtains
Transparent nanometer wood fibre film;
(2) after nanometer wood fibre film obtained in step (1) being impregnated in the six water nickel nitrate solutions of 3mol/L
It takes out and spontaneously dries, control nickel salt load capacity is the 50% of nanometer wood fibre total film mass.Then at tube furnace high temperature carbon
Change handles to obtain nickel carbon nano-fiber film material;Wherein, control carburizing temperature is 700 DEG C, and heating rate is 5 DEG C/min, is protected
Warm 2h, and it is passed through nitrogen protection;
(3) nickel carbon nano-fiber film material obtained in step (2) is placed in three electrode electrolysers and carries out constant potential
Method processing, then nickel-loaded/nickel oxide carbon nanofiber electrode material is obtained after being cleaned with ethyl alcohol and ultrapure water;Wherein,
Electrolyte in electrolytic cell uses the potassium hydroxide of 6mol/L, and control voltage is 0.8V, and sensitivity is set as 1.0e-1, when processing
Between be 500s.
The resistance value of the electrode material of the electrode material prepared in the present embodiment is lower, is 1 Ω, and specific capacitance is
115F/g。
Comparative example 1:
As shown in Figure 1, a kind of preparation method for the carbon nanofiber electrode material for loading nickel nickel, including following step
It is rapid:
(1) by 50g nanometer wood fibre (ultrapure water is solvent) (control nanometer wood fibre mass concentration be
0.5wt.%) risen at carbon nanometer wood fibre wherein control carburizing temperature is 700 DEG C after drying in the carbonization of tube furnace high temperature
Warm rate is 5 DEG C/min, keeps the temperature 2h, and be passed through nitrogen protection;
(2) carbon nanometer wood fibre obtained in step (1) is uniformly mixed with nickel nitrate, control nickel salt load capacity is total
The 30% of quality.Nickel carbon nano-fiber material is obtained then at tube furnace high temperature carbonization treatment;Wherein, control carburizing temperature is
800 DEG C, heating rate is 5 DEG C/min, keeps the temperature 2h, and be passed through nitrogen protection;
(3) nickel carbon nano-fiber material obtained in step (2) is placed in three electrode electrolysers and is carried out at potentiostatic method
Reason, then nickel-loaded/nickel oxide carbon nanofiber electrode material is obtained after being cleaned with ethyl alcohol and ultrapure water;Wherein, it is electrolysed
Electrolyte in slot uses the potassium hydroxide of 6mol/L, and control voltage is 1V, and sensitivity is set as 1.0e-1, processing the time be
100s。
The comparative example is that the electrode material can not be directly by nickel load in carbon fiber in the main distinction of above-described embodiment
On, while being difficult to form the electrode of full wafer, need to add the substances such as other binders, greatly affected its ion and electronics
Conduction, to influence chemical property.
Comparative example 2:
This comparative example compared with Example 1, the difference is that control when dispersing nanometer wood fibre in ultrapure water
The mass concentration of nanometer wood fibre solution is 1.0wt.%.
After measured, the resistance value of electrode is 2.7 Ω, specific capacitance 110F/g in this comparative example.
Claims (7)
1. a kind of preparation method for the carbon nanofiber electrode material for loading nickel nickel, which is characterized in that including following step
It is rapid:
(1) it disperses nanometer wood fibre in ultrapure water, nanometer wood fibre film is dried to obtain after vacuum filtration;
(2) nanometer wood fibre film obtained in step (1) is placed in nickel salt solution after impregnating and takes out drying, then pyrocarbon
Change handles to obtain nickel carbon nano-fiber film material;
(3) nickel carbon nano-fiber film material obtained in step (2) is handled by electroxidation and obtains nickel-loaded/oxidation
The carbon nanofiber electrode material of nickel.
2. preparation method according to claim 1, which is characterized in that the nanometer wood fibre passes through acid by cellulose powder
Hydrolysis-high pressure homogenization method is prepared;Nickel salt in the nickel salt solution is six water nickel chlorides, nickel sulfate hexahydrate or six water nitric acid
At least one of nickel.
3. preparation method according to claim 1 or 2, which is characterized in that control is carried on when impregnating in the step (2)
The quality of nickel salt on nanometer wood fibre film accounts for the 10%-70% of nickel carbon nano-fiber film material gross mass.
4. preparation method according to claim 3, which is characterized in that control, which is carried on, when impregnating in the step (2) receives
The quality of nickel salt on rice wood fibre film accounts for the 30%-60% of nickel carbon nano-fiber film material gross mass.
5. preparation method according to claim 1 or 2, which is characterized in that disperse nanometer wood fibre in ultrapure water
When control nanometer wood fibre solution mass concentration be 0.5-0.8wt.%.
6. preparation method according to claim 1 or 2, which is characterized in that high temperature cabonization processing in tube furnace,
It is carried out under nitrogen protection, and keeping carburizing temperature is 450-1000 DEG C, heating rate is 5-10 DEG C/min, soaking time 1-
3h。
7. preparation method according to claim 1 or 2, which is characterized in that the electroxidation processing is by nickel carbon Nanowire
Dimension thin-film material is placed in three-electrode system, then is handled using potentiostatic method, and electrolyte uses potassium hydroxide solution, control when processing
Voltage processed is 0.8-1.2V, and sensitivity is set as 1.0e-1, the processing time is 30-600s.
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