CN105590754A - Production method of multi-element transition metal hydroxide nuclear shell composite carbon filter electrode material - Google Patents
Production method of multi-element transition metal hydroxide nuclear shell composite carbon filter electrode material Download PDFInfo
- Publication number
- CN105590754A CN105590754A CN201610110092.8A CN201610110092A CN105590754A CN 105590754 A CN105590754 A CN 105590754A CN 201610110092 A CN201610110092 A CN 201610110092A CN 105590754 A CN105590754 A CN 105590754A
- Authority
- CN
- China
- Prior art keywords
- metal hydroxide
- fiber
- preparation
- nitrate
- polymer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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 OR LIGHT-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
-
- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a production method of a multi-element transition metal hydroxide nuclear shell composite carbon filter electrode material, and belongs to the electrode material production field. Nano-fibers can be produced by adopting the electrospinning method, and carbon fibers can be produced by adopting the high temperature carbonization method, and in addition, the surface functionalization can be realized by adopting the acid treatment, and the surface can be provided with the multi-element transition metal ions in a complexed manner, and then the in-situ growth transition metal hydroxide can be realized by adopting the base catalysis. The electrode material is advantageous in that the specific surface area of the nano-fiber film is large, and the porosity is high, and at the same time, the excellent electrochemistry performance is provided by combining with the high conductivity of the carbon fiber materials and the high capacitance of the multi-element metal hydroxide, and the important application value can be provided for the fields such as the lithium ion battery, the super capacitor, and other electronic devices.
Description
Technical field
The present invention relates to a kind of polynary transition metal hydroxide nucleocapsid carbon fiber reinforce plastic electrode materialPreparation method, belongs to the preparation field of electrode material.
Background technology
Along with day by day exhausted, the increasing environmental pollution of fossil energy, the environmentally friendly type of people efficientThe invention of energy storage device utilizes pay attention to day by day. Advanced energy storage and conversion system have developedCome, for example: lithium ion battery, ultracapacitor, solar cell, fuel cell. Wherein superCapacitor becomes one of a kind of main energy supply equipment, because it has high energy density, fastThe charge-discharge velocity of speed, long cycle life and eco-friendly feature.
Ionic adsorption and the desorption of electricity layer capacitor based on electrode surface is attached, cause having low electric capacity withEnergy density, fake capacitance utensil has better electrochemistry performance by contrast. Transiting metal oxidation recentlyThing or hydroxide NiO, RuO2, MnO2, Ni (OH) 2 grades are widely used in fake capacitance device electrodeMaterial, because its redox with high theoretical unit electric capacity and polyelectron faradic currents is anti-Should. But in the middle of actual application process due to transition metal oxide or the low conduction of hydroxideProperty, large Volume Changes, electric capacity decline fast and electrochemistry effect inferior in long oxidation reductionRate has limited its application. In order to address the above problem, with conduction material with carbon element be combined into for one canThe solution of energy, and obtained a large amount of research. Compared with other materials, material with carbon element has than tableArea is large, conductance is high, corrosion resistance is strong, have extended cycle life, lower-price characteristic, wherein livesProperty carbon fiber is the third generation product of active carbon material, is desirable electrode material. But currentIn research, be mainly by single metal oxides or hydroxide and the compound electrode material of preparing of carbon fiber, thisPlant electrode material and can effectively improve its chemical property. But polynary metallic hydrogen oxidation is found in researchThing has outstanding performance owing to having cooperative effect.
We adopt electrostatic spinning to prepare PAN nanofiber through high-temperature calcination preparation in the present inventionBecome carbon nano-fiber, this fiber has good electrical and thermal conductivity performance and high cyclical stability, logicalPeracid treatment is that its surface produces carboxyl and carbonyl, and then surface complexation metal ion, at base catalysis barUnder part, realize growth in situ metal hydroxides, successfully prepared a kind of polynary transition metal hydroxideNucleocapsid carbon fiber reinforce plastic electrode material. This method is simple, quick, efficient, prepared electrode materialMaterial has high practical value in ultracapacitor.
Summary of the invention
The object of the invention is to utilize this simple, fast and efficient method preparation of electrostatic spinningPAN nanofiber presoma, is prepared into carbon nano-fiber through high-temperature calcination, and this fiber hasGood electrical and thermal conductivity performance and high cyclical stability, by acid treatment be its surface produce carboxyl andCarbonyl, then, in metal inorganic salting liquid, drips base catalysis, realizes many metals of growth in situ hydrogen-oxygenCompound, has successfully prepared polynary transition metal hydroxide nucleocapsid compound carbon nanofiber electrode material.
To achieve these goals, the present invention adopts following concrete implementation step:
A preparation method for polynary transition metal hydroxide nucleocapsid carbon fiber reinforce plastic electrode material, itsBe characterised in that and comprise the following steps:
1) preparation of polymer nanofiber: polymer dissolution, in organic solvent, is mixed with to polymerizationThing solution, after it dissolves completely, injects spinning needle tubing spinning voltage 15-20KV is set, and receivesCarry out spinning apart from 15-20cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the nanofiber arriving after dry, be positioned overIn vacuum tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CCarbonization 1h, the carbon nano-fiber obtaining is processed 30min with the mixed solution of sulfuric acid and nitric acid;
3) situ catalytic growth mixed metal hydroxide: the carbon nano-fiber after acid treatment is immersed inIn ethanol solution, add wherein metal salt mixture, after adsorption, then dropwise addEnter aqueous slkali catalysis and generate mixed metal hydroxide.
Further, above-mentioned steps 1) in polymer be polyacrylonitrile, polystyrene or polyaniline,Organic solvent is DMF, and polymer solution concentration is 10wt%～20wt%.
Further, above-mentioned steps 3) in the slaine of using be zinc nitrate, cobalt nitrate, copper nitrate,Ferric nitrate, nickel nitrate, manganese nitrate, zinc acetate, cobalt acetate, Schweinfurt green, wrong sour iron, nickel acetate,In manganese acetate two kinds, alkali used is ammoniacal liquor, NaOH, potassium hydroxide etc., multi-element metalMixing molar ratio between nitrate is 1:1～1:5, and the adsorption time is 2～8h, aqueous slkaliConcentration is 5wt%～10wt%
Innovative point of the present invention is:
1) the present invention utilizes electrostatic spinning nano fiber to prepare carbon nano-fiber for presoma, thisMethod is simple and quick, efficient, the carbon nano-fiber good conductivity obtaining, and good stability, has certainMechanical strength and flexibility, and kept nanofiber high-specific surface area, the feature of high porosity,The growth transition metal hydroxide taking it as base material, can prevent multi-element transition metal oxides reunion,Variation with volume in the cyclic process of opposing electrochemistry.
2) compared with monometallic transition metal hydroxide before, polynary transition metal hydroxide is different, there is strong cooperative effect in matter structure, chemical property is more excellent.
3) method of this room temperature growth in situ is than traditional electrochemical deposition and high temperature hydrothermal growthMethod be more easy to realize and energy-conservation, prepared polynary transition metal hydroxide composite carbon nanometerTunica fibrosa, has important using value in electrochemical field.
Brief description of the drawings
Fig. 1 the present invention presses the prepared hydroxide/carbon fiber nucleocapsid combination electrode material of embodiment 1Scanning electron microscope (SEM) photograph, the porous rough surface that surface forms for mixed metal hydroxide nanoscale twins.
Fig. 2. (1) is the corresponding CV curve map of example 1, and (2) are that example 2 is correspondingCV curve map; All the other embodiment obtain extremely similarly curve map.
Detailed description of the invention
Embodiment 1
1) preparation of polymer nanofiber: PAN is dissolved in DMF, is mixed with 10wt%Polymer solution, after it dissolves completely, injects spinning needle tubing spinning voltage 20KV is set, and connectsReceive and carry out spinning apart from 15cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the polymer fiber obtaining, be positioned over trueIn empty tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CHigh temperature cabonization 1h, the mixed solution (mol ratio 1:1) of sulfuric acid and nitric acid for the carbon nano-fiber obtainingProcess 30min;
3) situ catalytic growth mixed metal hydroxide: by the carbon nanometer fibre obtaining in above-mentioned stepsDimension, cuts 2cm*2cm and is immersed in 20ml ethanol solution, adds wherein 2g mol ratioFor zinc nitrate/cobalt nitrate mixture of 1:1, surface dissolution absorption 2h, then dropwise adds 25g'sThe catalysis of the 5wt%KOH aqueous solution generates mixed metal hydroxide.
Embodiment 2
1) preparation of polymer nanofiber: PAN is dissolved in DMF, is mixed with 15wt%Polymer solution, after it dissolves completely, injects spinning needle tubing spinning voltage 15KV is set, and connectsReceive and carry out spinning apart from 15cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the polymer fiber obtaining, be positioned over trueIn empty tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CHigh temperature cabonization 1h, the mixed solution (mol ratio 1:1) of sulfuric acid and nitric acid for the carbon nano-fiber obtainingProcess 30min;
3) situ catalytic growth mixed metal hydroxide: by the carbon nanometer fibre obtaining in above-mentioned stepsDimension, cuts 2cm*2cm and is immersed in 20ml ethanol solution, adds wherein 2g mol ratioFor zinc nitrate/cobalt nitrate mixture of 1:2, surface dissolution absorption 4h, then dropwise adds 18g'sThe catalysis of the 7wt%KOH aqueous solution generates mixed metal hydroxide.
Embodiment 3
1) preparation of polymer nanofiber: PAN is dissolved in DMF, is mixed with 15wt%Polymer solution, after it dissolves completely, injects spinning needle tubing spinning voltage 20KV is set, and connectsReceive and carry out spinning apart from 20cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the polymer fiber obtaining, be positioned over trueIn empty tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CHigh temperature cabonization 1h, the mixed solution (mol ratio 1:1) of sulfuric acid and nitric acid for the carbon nano-fiber obtainingProcess 30min;
3) situ catalytic growth mixed metal hydroxide: by the carbon nanometer fibre obtaining in above-mentioned stepsDimension, cuts 2cm*2cm and is immersed in 20ml ethanol solution, adds wherein 2g mol ratioFor zinc nitrate/cobalt nitrate mixture of 1:3, surface dissolution absorption 6h, then dropwise adds 15g'sThe catalysis of the 9wt%KOH aqueous solution generates mixed metal hydroxide.
Embodiment 4
1) preparation of polymer nanofiber: PAN is dissolved in DMF, is mixed with 12wt%Polymer solution, after it dissolves completely, injects spinning needle tubing spinning voltage 20KV is set, and connectsReceive and carry out spinning apart from 15cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the polymer fiber obtaining, be positioned over trueIn empty tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CHigh temperature cabonization 1h, the mixed solution (mol ratio 1:1) of sulfuric acid and nitric acid for the carbon nano-fiber obtainingProcess 30min;
3) situ catalytic growth mixed metal hydroxide: by the carbon nanometer fibre obtaining in above-mentioned stepsDimension, cuts 2cm*2cm and is immersed in 20ml ethanol solution, adds wherein 2g mol ratioFor zinc nitrate/cobalt nitrate mixture of 1:4, surface dissolution absorption 4h, then dropwise adds 16g'sThe catalysis of 5wt% ammonia spirit generates mixed metal hydroxide.
Embodiment 5
1) preparation of polymer nanofiber: PAN is dissolved in DMF, is mixed with 13wt%Polymer solution, after it dissolves completely, injects spinning needle tubing spinning voltage 20KV is set, and connectsReceive and carry out spinning apart from 15cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the polymer fiber obtaining, be positioned over trueIn empty tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CHigh temperature cabonization 1h, the mixed solution (mol ratio 1:1) of sulfuric acid and nitric acid for the carbon nano-fiber obtainingProcess 30min;
3) situ catalytic growth mixed metal hydroxide: by the carbon nanometer fibre obtaining in above-mentioned stepsDimension, cuts 2cm*2cm and is immersed in 20ml ethanol solution, adds wherein 2g mol ratioFor manganese nitrate/cobalt nitrate mixture of 1:1, surface dissolution absorption 5h, then dropwise adds 8g'sThe catalysis of 10wt% ammonia spirit generates mixed metal hydroxide.
Embodiment 6
1) preparation of polymer nanofiber: PAN is dissolved in DMF, is mixed with 14wt%Polymer solution, after it dissolves completely, injects spinning needle tubing spinning voltage 20KV is set, and connectsReceive and carry out spinning apart from 15cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the polymer fiber obtaining, be positioned over trueIn empty tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CHigh temperature cabonization 1h, the mixed solution (mol ratio 1:1) of sulfuric acid and nitric acid for the carbon nano-fiber obtainingProcess 30min;
3) situ catalytic growth mixed metal hydroxide: by the carbon nanometer fibre obtaining in above-mentioned stepsDimension, cuts 2cm*2cm and is immersed in 20ml ethanol solution, adds wherein 2g mol ratioFor manganese nitrate/cobalt nitrate mixture of 1:5, surface dissolution absorption 2h, then dropwise adds 22g'sThe catalysis of 5wt% sodium hydrate aqueous solution generates mixed metal hydroxide.
Embodiment 7
1) preparation of polymer nanofiber: PAN is dissolved in DMF, is mixed with 10wt%Polymer solution, after it dissolves completely, injects spinning needle tubing spinning voltage 20KV is set, and connectsReceive and carry out spinning apart from 15cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the polymer fiber obtaining, be positioned over trueIn empty tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CHigh temperature cabonization 1h, the mixed solution (mol ratio 1:1) of sulfuric acid and nitric acid for the carbon nano-fiber obtainingProcess 30min;
3) situ catalytic growth mixed metal hydroxide: by the carbon nanometer fibre obtaining in above-mentioned stepsDimension, cuts 2cm*2cm and is immersed in 20ml ethanol solution, adds wherein 2g mol ratioFor nickel nitrate/cobalt nitrate mixture of 1:1, surface dissolution absorption 2h, then dropwise adds 25g'sThe catalysis of the 5wt%KOH aqueous solution generates mixed metal hydroxide.
Embodiment 8
1) preparation of polymer nanofiber: PAN is dissolved in DMF, is mixed with 10wt%Polymer solution, after it dissolves completely, injects spinning needle tubing spinning voltage 20KV is set, and connectsReceive and carry out spinning apart from 15cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the polymer fiber obtaining, be positioned over trueIn empty tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CHigh temperature cabonization 1h, the mixed solution (mol ratio 1:1) of sulfuric acid and nitric acid for the carbon nano-fiber obtainingProcess 30min;
3) situ catalytic growth mixed metal hydroxide: by the carbon nanometer fibre obtaining in above-mentioned stepsDimension, cuts 2cm*2cm and is immersed in 20ml ethanol solution, adds wherein 2g mol ratioFor copper nitrate/cobalt nitrate mixture of 1:1, surface dissolution absorption 2h, then dropwise adds 25g'sThe catalysis of the 5wt%KOH aqueous solution generates mixed metal hydroxide.
Embodiment 9
1) preparation of polymer nanofiber: PAN is dissolved in DMF, is mixed with 10wt%Polymer solution, after it dissolves completely, injects spinning needle tubing spinning voltage 20KV is set, and connectsReceive and carry out spinning apart from 15cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the polymer fiber obtaining, be positioned over trueIn empty tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CHigh temperature cabonization 1h, the mixed solution (mol ratio 1:1) of sulfuric acid and nitric acid for the carbon nano-fiber obtainingProcess 30min;
3) situ catalytic growth mixed metal hydroxide: by the carbon nanometer fibre obtaining in above-mentioned stepsDimension, cuts 2cm*2cm and is immersed in 20ml ethanol solution, adds wherein 2g mol ratioFor zinc nitrate/nickel nitrate mixture of 1:1, surface dissolution absorption 2h, then dropwise adds 25g's5wt%KOH solution catalyzing generates mixed metal hydroxide.
Embodiment 10
1) preparation of polymer nanofiber: PAN is dissolved in DMF, is mixed with 20wt%Polymer solution, after it dissolves completely, injects spinning needle tubing spinning voltage 20KV is set, and connectsReceive and carry out spinning apart from 15cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the polymer fiber obtaining, be positioned over trueIn empty tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CHigh temperature cabonization 1h, the mixed solution (mol ratio 1:1) of sulfuric acid and nitric acid for the carbon nano-fiber obtainingProcess 30min;
3) situ catalytic growth mixed metal hydroxide: by the carbon nanometer fibre obtaining in above-mentioned stepsDimension, cuts 2cm*2cm and is immersed in 20ml ethanol solution, adds wherein 2g mol ratioFor zinc nitrate/cobalt nitrate mixture of 1:5, surface dissolution absorption 8h, then dropwise adds 13g's10wt%KOH solution catalyzing generates mixed metal hydroxide.
Embodiment 11
1) preparation of polymer nanofiber: PS is dissolved in DMF, is mixed with 10wt% poly-Compound solution, after it dissolves completely, injects spinning needle tubing spinning voltage 20KV is set, and receivesCarry out spinning apart from 15cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the polymer fiber obtaining, be positioned over trueIn empty tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CHigh temperature cabonization 1h, the mixed solution (mol ratio 1:1) of sulfuric acid and nitric acid for the carbon nano-fiber obtainingProcess 30min;
3) situ catalytic growth mixed metal hydroxide: by the carbon nanometer fibre obtaining in above-mentioned stepsDimension, cuts 2cm*2cm and is immersed in 20ml ethanol solution, adds wherein 2g mol ratioFor zinc nitrate/nickel nitrate mixture of 1:1, surface dissolution absorption 2h, then dropwise adds 25g's5wt%KOH solution catalyzing generates mixed metal hydroxide.
Embodiment 12
1) preparation of polymer nanofiber: PANI is dissolved in DMF, is mixed with 10wt%Polymer solution, after it dissolves completely, injects spinning needle tubing spinning voltage 20KV is set, and connectsReceive and carry out spinning apart from 15cm, the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the polymer fiber obtaining, be positioned over trueIn empty tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, and then nitrogen atmosphere is warming up to 1000 DEG CHigh temperature cabonization 1h, the mixed solution (mol ratio 1:1) of sulfuric acid and nitric acid for the carbon nano-fiber obtainingProcess 30min;
3) situ catalytic growth mixed metal hydroxide: by the carbon nanometer fibre obtaining in above-mentioned stepsDimension, cuts 2cm*2cm and is immersed in 20ml ethanol solution, adds wherein 2g mol ratioFor zinc nitrate/nickel nitrate mixture of 1:1, surface dissolution absorption 2h, then dropwise adds 25g's5wt%KOH solution catalyzing generates mixed metal hydroxide.
Claims (3)
1. a preparation method for polynary transition metal hydroxide nucleocapsid carbon fiber reinforce plastic electrode material, is characterized in that comprising the following steps:
1) preparation of polymer nanofiber: by polymer dissolution in organic solvent, be mixed with polymer solution, after it dissolves completely, inject spinning needle tubing spinning voltage 15-20KV is set, receiving range 15-20cm carries out spinning, and the nanofiber obtaining is dry 24h in vacuum drying chamber;
2) preparation of surface-functionalized carbon nano-fiber: by the nanofiber arriving after dry, be positioned in vacuum tube furnace, air atmosphere is through 280 DEG C of pre-oxidation 2h, then nitrogen atmosphere is warming up to 1000 DEG C of carbonization 1h, and the carbon nano-fiber obtaining is processed 30min with the mixed solution of sulfuric acid and nitric acid;
3) situ catalytic growth mixed metal hydroxide: the carbon nano-fiber after acid treatment is immersed in ethanol solution, adds wherein metal salt mixture, after adsorption, then dropwise add aqueous slkali catalysis to generate mixed metal hydroxide.
2. preparation method according to claim 1, is characterized in that above-mentioned steps 1) in polymer be polyacrylonitrile, polystyrene or polyaniline, organic solvent is DMF, polymer solution concentration is 10wt%～20wt%.
3. preparation method according to claim 1, it is characterized in that above-mentioned steps 3) in the slaine of using be zinc nitrate, cobalt nitrate, copper nitrate, ferric nitrate, nickel nitrate, manganese nitrate, zinc acetate, cobalt acetate, Schweinfurt green, wrong sour iron, nickel acetate, in manganese acetate two kinds, alkali used is ammoniacal liquor, NaOH or potassium hydroxide, mixing molar ratio between multi-element metal nitrate is 1:1～1:5, and the adsorption time is 2～8h, and the concentration of aqueous slkali is 5wt%～10wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610110092.8A CN105590754A (en) | 2016-02-27 | 2016-02-27 | Production method of multi-element transition metal hydroxide nuclear shell composite carbon filter electrode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610110092.8A CN105590754A (en) | 2016-02-27 | 2016-02-27 | Production method of multi-element transition metal hydroxide nuclear shell composite carbon filter electrode material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105590754A true CN105590754A (en) | 2016-05-18 |
Family
ID=55930251
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610110092.8A Pending CN105590754A (en) | 2016-02-27 | 2016-02-27 | Production method of multi-element transition metal hydroxide nuclear shell composite carbon filter electrode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105590754A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106229162A (en) * | 2016-08-05 | 2016-12-14 | 宁波金特信钢铁科技有限公司 | A kind of preparation method of transition metal carbon nano-composite material |
| CN106847529A (en) * | 2017-01-21 | 2017-06-13 | 中国科学院深圳先进技术研究院 | Combination electrode material and preparation method thereof |
| CN107293408A (en) * | 2017-06-01 | 2017-10-24 | 大连理工大学 | A kind of nickel cobalt hydroxide/nitrogenous activated carbon composite electrode material and preparation method thereof |
| CN107565106A (en) * | 2017-07-27 | 2018-01-09 | 中国科学技术大学 | The preparation method of graphene quantum dot and the composite nano-line of ferrimanganic solid solution |
| CN107633959A (en) * | 2017-08-29 | 2018-01-26 | 深圳技术大学筹备办公室 | A kind of preparation method of electrode material |
| CN107658140A (en) * | 2017-08-07 | 2018-02-02 | 南昌大学 | The structure and preparation method of a kind of self-supporting super capacitor electrode material |
| CN109273278A (en) * | 2018-10-23 | 2019-01-25 | 陕西科技大学 | A kind of preparation method of cobalt acid nickel nano wire cladding carbon fiber flexible electrode material |
| CN109449011A (en) * | 2018-10-23 | 2019-03-08 | 陕西科技大学 | A kind of preparation method growing needle-shaped network structure cobalt acid nickel flexible electrode using carbon fiber as supporter |
| CN109637844A (en) * | 2018-11-27 | 2019-04-16 | 中国电子科技集团公司第十八研究所 | Preparation method of positive electrode composite material for lithium ion capacitor |
| CN110551443A (en) * | 2019-10-24 | 2019-12-10 | 武建云 | Waterborne polyurethane environment-friendly conductive coating and preparation method thereof |
| CN113213589A (en) * | 2021-04-28 | 2021-08-06 | 华南理工大学 | Three-metal carbon nanofiber loaded electro-Fenton cathode and preparation method and application thereof |
| CN115627018A (en) * | 2022-10-26 | 2023-01-20 | 江苏创合橡塑有限公司 | Preparation method of ageing-resistant high-elasticity rubber compound |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103426649A (en) * | 2013-08-21 | 2013-12-04 | 吉林大学 | Preparation method for different carbon fibers / cobalt hydroxide electrode and solid-liquid composite electrode system |
| CN104392847A (en) * | 2014-09-24 | 2015-03-04 | 黑龙江大学 | Preparation method of morphology controllable metal oxide/active carbon fiber combination electrode material |
-
2016
- 2016-02-27 CN CN201610110092.8A patent/CN105590754A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103426649A (en) * | 2013-08-21 | 2013-12-04 | 吉林大学 | Preparation method for different carbon fibers / cobalt hydroxide electrode and solid-liquid composite electrode system |
| CN104392847A (en) * | 2014-09-24 | 2015-03-04 | 黑龙江大学 | Preparation method of morphology controllable metal oxide/active carbon fiber combination electrode material |
Non-Patent Citations (2)
| Title |
|---|
| FEILI LAI, ET AL.: ""Controllable preparation of multi-dimensional hybrid materials of nickel-cobalt layered double hydroxide nanorods/nanosheets on electrospun carbon nanofibers for high-performance supercapacitors"", 《ELECTROCHIMICA ACTA》 * |
| LONGSHENG ZHANG,ET AL.: ""Flexible Hybrid Membranes with Ni(OH)2 Nanoplatelets Vertically Grown on Electrospun Carbon Nanofibers for High-Performance Supercapacitors"", 《ACS APPL. MATER. INTERFACES》 * |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106229162B (en) * | 2016-08-05 | 2018-07-06 | 威海南海碳材料有限公司 | A kind of preparation method of transition metal carbon nano-composite material |
| CN106229162A (en) * | 2016-08-05 | 2016-12-14 | 宁波金特信钢铁科技有限公司 | A kind of preparation method of transition metal carbon nano-composite material |
| CN106847529A (en) * | 2017-01-21 | 2017-06-13 | 中国科学院深圳先进技术研究院 | Combination electrode material and preparation method thereof |
| CN107293408A (en) * | 2017-06-01 | 2017-10-24 | 大连理工大学 | A kind of nickel cobalt hydroxide/nitrogenous activated carbon composite electrode material and preparation method thereof |
| CN107293408B (en) * | 2017-06-01 | 2019-03-05 | 大连理工大学 | A kind of nickel cobalt hydroxide/nitrogenous activated carbon composite electrode material and preparation method thereof |
| CN107565106A (en) * | 2017-07-27 | 2018-01-09 | 中国科学技术大学 | The preparation method of graphene quantum dot and the composite nano-line of ferrimanganic solid solution |
| CN107658140A (en) * | 2017-08-07 | 2018-02-02 | 南昌大学 | The structure and preparation method of a kind of self-supporting super capacitor electrode material |
| CN107633959A (en) * | 2017-08-29 | 2018-01-26 | 深圳技术大学筹备办公室 | A kind of preparation method of electrode material |
| CN109273278A (en) * | 2018-10-23 | 2019-01-25 | 陕西科技大学 | A kind of preparation method of cobalt acid nickel nano wire cladding carbon fiber flexible electrode material |
| CN109449011A (en) * | 2018-10-23 | 2019-03-08 | 陕西科技大学 | A kind of preparation method growing needle-shaped network structure cobalt acid nickel flexible electrode using carbon fiber as supporter |
| CN109637844A (en) * | 2018-11-27 | 2019-04-16 | 中国电子科技集团公司第十八研究所 | Preparation method of positive electrode composite material for lithium ion capacitor |
| CN110551443A (en) * | 2019-10-24 | 2019-12-10 | 武建云 | Waterborne polyurethane environment-friendly conductive coating and preparation method thereof |
| CN113213589A (en) * | 2021-04-28 | 2021-08-06 | 华南理工大学 | Three-metal carbon nanofiber loaded electro-Fenton cathode and preparation method and application thereof |
| CN113213589B (en) * | 2021-04-28 | 2022-03-29 | 华南理工大学 | Three-metal carbon nanofiber loaded electro-Fenton cathode and preparation method and application thereof |
| CN115627018A (en) * | 2022-10-26 | 2023-01-20 | 江苏创合橡塑有限公司 | Preparation method of ageing-resistant high-elasticity rubber compound |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105590754A (en) | Production method of multi-element transition metal hydroxide nuclear shell composite carbon filter electrode material | |
| Xiong et al. | A high-performance hybrid supercapacitor with NiO derived NiO@ Ni-MOF composite electrodes | |
| Shi et al. | Flexible 3D carbon cloth as a high-performing electrode for energy storage and conversion | |
| CN103337639B (en) | Preparation method of carbon nano tube array/carbon fiber fabric integrated three-dimensional porous air electrode | |
| CN102683037B (en) | Manganese dioxide asymmetric super-capacitor and preparation method thereof | |
| CN107359054B (en) | Composite electrode material, preparation method and application thereof | |
| CN108922790B (en) | Preparation method and application of composite material | |
| CN104392847B (en) | Preparation method of morphology controllable metal oxide/active carbon fiber combination electrode material | |
| CN100541688C (en) | Preparation method of expanded graphite/metal oxide composite material | |
| CN102087921A (en) | Self-supporting super capacitor electrode material and preparation method thereof | |
| CN103762091A (en) | Cellular porous manganese dioxide nanofiber preparing method and application of cellular porous manganese dioxide nanofiber in supercapacitor | |
| CN104973596A (en) | Hetero atom-doped hollow spherical grapheme composite material, and preparation method and applications thereof | |
| CN103545116A (en) | Foamed nickel-nanometer eight-vulcanization and nine-cobalt composite material, preparation method for same and super-capacitor electrode | |
| CN106430146A (en) | Nitrogen-manganese co-doped hierarchical porous carbon material preparation method | |
| CN107201573A (en) | A kind of preparation method and applications of cobalt disulfide and carbon nano-fiber composite material | |
| CN107863536A (en) | Multiple dimensioned porous electrode applied to flow battery and its preparation method and application | |
| CN109741966B (en) | Ni6MnO8@ carbon nanotube composite material and preparation method and application thereof | |
| CN104715936A (en) | Hierarchical porous carbon electrode material for supercapacitor and preparation method | |
| Tang et al. | Enhancement in electrochemical performance of nitrogen-doped hierarchical porous carbon-based supercapacitor by optimizing activation temperature | |
| Liu et al. | The CuCo2O4/CuO composite-based microspheres serve as a battery-type cathode material for highly capable hybrid supercapacitors | |
| CN110517900A (en) | A kind of preparation method of supercapacitor N doping low temperature carbon nanofiber electrode material | |
| CN106683894A (en) | Co3O4 porous nanosheet array preparation method and application thereof | |
| CN107170588A (en) | A kind of carbon-nitrogen doped cobalt aluminum oxide composite material and preparation method thereof | |
| CN112726192B (en) | Preparation method of electrospun carbon nanofiber/reduced graphene oxide/polyaniline/basic nickel carbonate composite electrode material | |
| CN101872651B (en) | Method for preparing in-situ self-grown nano carbon composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160518 |