CN106876733A - A kind of CNT self-assembled nanometer fibrofelt and its preparation and application - Google Patents
A kind of CNT self-assembled nanometer fibrofelt and its preparation and application Download PDFInfo
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- CN106876733A CN106876733A CN201510926445.7A CN201510926445A CN106876733A CN 106876733 A CN106876733 A CN 106876733A CN 201510926445 A CN201510926445 A CN 201510926445A CN 106876733 A CN106876733 A CN 106876733A
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/96—Carbon-based electrodes
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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
- H01M4/00—Electrodes
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- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
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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
- H01M4/00—Electrodes
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- H01M4/88—Processes of manufacture
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
- H01M8/184—Regeneration by electrochemical means
- H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
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Abstract
The invention discloses a kind of CNT self-assembled nanometer fibrofelt and its preparation and the application in all-vanadium flow battery, CNT self-assembled nanometer fibrofelt is based on CNT, high molecular polymer is assembling agent, it is made through method of electrostatic spinning, in 100-1000nm, specific surface area is 30-1000m to the wherein diameter of fiber2.g-1, porosity is more than 90%.Carbon nano-fiber felt material prepared by the preparation method is used for vanadium redox flow battery electrode, shows excellent chemical property, with processability is excellent, process is simple, good process repeatability, low cost and advantages of environment protection.
Description
Technical field
The present invention relates to a kind of preparation method and applications of carbon material, particularly a kind of CNT self assembly is received
Rice fibrous felt materials and its application on all-vanadium flow battery
Background technology
The energy and environment are the two large problems of 21 century facing mankind.With continuing to develop for economic society, people
Class is increasing to the demand of the energy.But traditional fossil energy one side reserves are limited, it is impossible to meet society
The demand that can develop, consuming excessively for another aspect fossil energy brings serious environmental problem.To understand
The certainly dual problem of energy shortage and environmental pollution, reproducible clean energy resource, such as solar energy and wind energy are opened
Send out most important.But, the characteristics of solar power generation and wind power generation have discontinuous unstable, by nature
Ambient influnence is larger.Because extensive energy storage technology can solve the problem that this problem, so it is subject to widely studied.
Wherein all-vanadium flow battery technology has led the development of battery industry with its unique advantage, and is widely used.
The electrode material of all-vanadium flow battery is one of critical material in liquid flow energy storage battery, and its own is without work
Property material, do not react, but for dissolving active material in the liquid phase provides the place reacted, battery exists
Electrode material surface completes the conversion between electric energy-chemical energy.For all-vanadium flow system, battery both sides occur
Reaction have：
Positive pole：VO2++2H++e-=VO2++H2O
Negative pole：V3++e-=V2+。
All-vanadium flow system requirement electrode material has following performance：1. high catalytic activity, to both sides redox
Electricity is to good activity and invertibity, reducing the activation polarization of battery；2. high-specific surface area, is anti-
More active sites should be provided；3. good electron conduction, advantageously reduces the ohmic internal resistance of battery；Compared with
Big porosity and surface has hydrophily, is easy to the diffusion transport of electrolyte, reduces the concentration polarization of battery
Change.4. good mechanical performance and corrosion resistance, washing away for fluid-resistant can be in the environment of strong acid Strong oxdiative
Keep stabilization.5. with low cost.
VRB electrode materials are generally divided into two classes：Metal class electrode and carbon class electrode.People's trial gold,
Lead, titanium, titanium-based platinum and titanium-based yttrium oxide etc. are used as VRB electrode materials.VO2+/VO2+ electricity is on gold electrode
Show electrochemical reaction irreversibility.Lead electrode and Ti electrode then easily in Surface Creation passivating film, cause
Resistance increase is unfavorable for further carrying out for reaction.Titanium-based platinum electrode avoids Ti electrode Surface Creation passivating film
Problem, show preferable electro-chemical activity in both positive and negative polarity.Titanium-based yttrium oxide (DSA) electrode have compared with
Invertibity high.But high cost limits the large-scale application of both electrodes.Carbon class electrode material species
It is various, including carbon paper, carbon cloth, carbon felt, CNT etc..This kind of electrode material electrical conductivity is higher, chemistry,
Electrochemical stability is good, and raw material sources enrich, moderate, is current comparatively ideal VRB electrode materials.
Wherein CNT has just showed the electrochemical stability of brilliance, but CNT is generally powder, it is difficult to use
In practical application.
The content of the invention
It is an object of the invention to provide a kind of CNT self-assembled nanometer fibrofelt and its preparation and application.
To achieve the above object, the technical scheme that the present invention is used is as follows：
A kind of CNT self-assembled nanometer fibrofelt, based on CNT, high molecular polymer is assembling
Agent, is made through method of electrostatic spinning, and in 100-1000nm, specific surface area is 30-1000 to the wherein diameter of fiber
㎡.g-1, porosity is more than 90%；
Described high molecular polymer be polyvinylpyrrolidone, polyacrylonitrile, PLA, Kynoar,
Polyvinyl alcohol, one or more in polymethyl methacrylate.
The specific preparation method of its carbon nano-fiber felt material is as follows：
CNT is scattered in solvent, ultrasound makes its dispersed in 1 hour, configures carbon nano tube dispersion liquid；
High molecular polymer is dissolved in above-mentioned dispersion liquid, 10-30h is stirred at 40-85 DEG C makes it fully molten
Solution, prepares CNT spinning solution；
Spinning solution dries 24h through electrostatic spinning into carbon nano-tube fibre film at being placed on 110 DEG C, is inciting somebody to action
1-3h is pre-oxidized in air at 200-350 DEG C to polymer fiber film, then under nitrogen or argon in
800-1400 DEG C of sintering 1-3h, dries；
Spinning solution is into the process of carbon nano-tube fibre film through electrostatic spinning：Respectively by the different high scores of 3-50mL
Sub- polymer solution is placed in different syringes, keeps syringe needle point with receiver board in 5-20cm distances,
From syringe needle point and voltage 10-30KV, 10-30 DEG C, relative humidity 10%-40% bars of receiver board
Part carries out spinning；
Between 10-80nm, high molecular polymer is polyvinylpyrrolidone to described carbon nanotube diameter, is gathered
Acrylonitrile, PLA, Kynoar, polyvinyl alcohol, one or two in polymethyl methacrylate
More than；
The mass fraction of CNT is 3-20% in the spinning solution, and the mass fraction of high molecular polymer is
2%-10%；
One kind or several in the solvent N,N-dimethylformamide, absolute ethyl alcohol, tetrahydrofuran, dichloromethane
Kind.
Beneficial effects of the present invention：
1. the CNT self-assembled nanometer fibrous felt materials that the present invention is provided are prepared with method of electrostatic spinning
, raw material is easy to get, cheap, it is easy to mass produce.
2. the CNT self-assembled nanometer fibrous felt materials that the present invention is provided can directly obtain felted material
Material, is directly used in electrode, it is to avoid subsequent electrode preparation process, simplifies experimental procedure, while avoiding
The use of binding agent, reduces side reaction.
3. the CNT self-assembled nanometer fibrous felt materials that the present invention is provided have very big porosity, are
Liquid flowing provides good passage, with excellent mass transfer ability.
4. the CNT self-assembled nanometer fibrous felt materials that prepared by preparation method of the present invention are used for complete
Vanadium flow battery electrode material, shows excellent chemical property, and steady with good circulation
It is qualitative.
Brief description of the drawings
Fig. 1 is the SEM pictures of the CNT self-assembled nanometer fibrous felt materials that embodiment 1 is obtained.
Fig. 2 is that the CNT self-assembled nanometer fibrous felt materials that embodiment 2 is obtained are electric as all-vanadium flow battery
The cycle performance curve of pole material.
Specific embodiment
With reference to embodiment, the invention will be further described, but implementation of the invention is not limited only to this.
The assemble method of all-vanadium flow battery is as follows in following examples：
At room temperature, all-vanadium flow battery is assembled in glove box.Collector plate is graphite cake, in graphite cake
On be carved with flow field for the flowing of electrolyte provides passage.It is electricity to use Nafion115 types cation-exchange membrane
Pond barrier film, film effective area be 9cm-2.Vanadium ion concentration is 1.50mol L in electrolyte-1, H2SO4
Concentration is 3mol L-1.
All-vanadium flow battery electrochemical test method is as follows in following examples：
At room temperature, the all-vanadium flow battery that will be assembled is in 40mA cm-2Current density carry out charge-discharge test.
Charge and discharge system is constant current charge-discharge, and it is 1.65-1.0V that discharge and recharge is interval.Charging-discharge tester system is ARBIN.
Embodiment 1
From diameter 20nm, the CNT of certain mass is scattered in N, N- by the CNT that 20 μm of length
In dimethyl formamide solution, ultrasound 30 minutes configures carbon nano tube dispersion liquid, by poly- the third of certain mass
Alkene nitrile powder is dissolved in dispersion liquid, and wherein the mass fraction of CNT is 7.5%, the quality point of polyacrylonitrile
Number 7.5%, at 60 DEG C stirring 8h makes it fully dissolve to obtain dispersed solution.Then by 10mL
Above-mentioned solution be placed in syringe, in 10KV voltages, 25 DEG C, carried out under conditions of relative humidity 30%
Spinning, syringe needle point is 5cm with the distance of receiver board.The polymer fiber felt that will be obtained is placed in 110 DEG C
Lower drying 10h, the polymer fiber felt that will be obtained pre-oxidizes 2h at 300 DEG C in air, then in argon gas
1h is sintered in 1000 DEG C under atmosphere, is dried.CNT self-assembled nanometer fibrous material as shown in Figure 1
SEM image show that it is interlocked by CNT self assembly and form that wherein the fiber of CNT composition is straight
Footpath forms abundant macroporous structure between 700nm or so, carbon fiber, and (specific surface area is 500 ㎡ .g-1,
Porosity is conducive to the raising of mass-transfer performance 90%).
Embodiment 2
From diameter 30nm, the CNT of certain mass is scattered in N, N- by the CNT that 15 μm of length
In dimethyl formamide solution, ultrasound 30 minutes configures carbon nano tube dispersion liquid, by the poly- first of certain mass
Base methyl acrylate powder is dissolved in dispersion liquid, and wherein the mass fraction of CNT is 10%, polymethyl
The mass fraction 5% of sour methyl esters, at 50 DEG C stirring 24h makes it fully dissolve to obtain dispersed solution.
Then the above-mentioned solution of 10mL is placed in syringe, in 15KV voltages, 25 DEG C, relative humidity 10%
Under conditions of carry out spinning, syringe needle point is 5cm with the distance of receiver board.The polymer fiber that will be obtained
Felt dries 10h at being placed in 110 DEG C, and the polymer fiber felt that will be obtained pre-oxidizes 2h at 300 DEG C in air,
Then 1h is sintered in 1000 DEG C under an argon atmosphere, is dried.The nano-sized carbon prepared using the present invention in Fig. 2
Fibrous felt materials show excellent chemical property as the electrode material of all-vanadium flow battery：In 20mA
cm-2, 40mA cm-2, 60mA cm-2Under the conditions of discharge and recharge 92%, 88% can be reached respectively with voltage efficiency,
81%, illustrate that the carbon nano-fiber felt material of present invention preparation shows excellent electricity in all-vanadium flow battery
Chemical property.
Embodiment 3
From diameter 30nm, the CNT of certain mass is scattered in N, N- by the CNT that 15 μm of length
In dimethyl formamide solution, ultrasound 30 minutes configures carbon nano tube dispersion liquid, by the poly- breast of certain mass
Sour powder is dissolved in dispersion liquid, and wherein the mass fraction of CNT is 5%, the mass fraction 5% of PLA,
12h is stirred at 55 DEG C to be made it fully dissolve to obtain dispersed solution.Then by above-mentioned the two of 15mL
Plant solution to be respectively placed in syringe, in 20KV voltages, 25 DEG C, carried out under conditions of relative humidity 15%
Spinning, syringe needle point is 10cm with the distance of receiver board.The polymer fiber felt that will be obtained is at 300 DEG C
3h is pre-oxidized in air, then 2h is sintered in 800 DEG C under an argon atmosphere, dried.Gained carbon nanometer
The diameter of fiber forms abundant macroporous structure between 800nm or so, carbon fiber and (compares table in pipe fibrofelt
Area is 500 ㎡ .g-1, 91%) porosity is.
Claims (6)
1. a kind of CNT self-assembled nanometer fibrofelt, it is characterised in that：The nanofiber mats are with carbon
Nanotube is main body, high molecular polymer is assembling agent, is prepared from through method of electrostatic spinning, wherein fiber
In 100-1000nm, specific surface area is 30-1000 ㎡ .g to diameter-1, porosity is more than 90%；
Described carbon nanotube diameter is 10-80nm, and high molecular polymer is polyvinylpyrrolidone, polypropylene
One or more in nitrile, PLA, Kynoar, polyvinyl alcohol, polymethyl methacrylate.
2. according to nanofiber mats described in claim 1, it is characterised in that：The porosity is in 90-95%；
Carbon nanotube diameter length is 0.5-30 μm；CNT is 3-20 with high molecular polymer mass ratio:2-10.
3. the preparation method of the CNT self-assembled nanometer fibrofelt described in a kind of claim 1 or 2, its
It is characterised by：Preparation process is as follows,
CNT is scattered in solvent, ultrasound makes its dispersed in more than 1 hour, configuration CNT point
Dispersion liquid；
High molecular polymer is dissolved in above-mentioned dispersion liquid, 10-30h is stirred at 40-85 DEG C makes it fully molten
Solution, prepares CNT spinning solution；
Spinning solution dries 12-48h through electrostatic spinning into carbon nano-tube fibre film at being placed on 100-120 DEG C,
1-3h is pre-oxidized in air at 200-350 DEG C polymer fiber film will be obtained, then in nitrogen and/or
1-3h is sintered in 800-1400 DEG C under argon gas, is dried；
Spinning solution is into the process of carbon nano-tube fibre film through electrostatic spinning：Spinning solution is placed in syringe, is protected
Syringe needle point is held with receiver board in 5-20cm distances, from syringe needle point and the voltage 10-30 of receiver board
KV, 10-30 DEG C, relative humidity 10%-40% conditions carry out spinning.
4. preparation method according to claim 3, it is characterised in that：Described carbon nanotube diameter is
10-80nm, length is 0.5-30 μm, and high molecular polymer is polyvinylpyrrolidone, polyacrylonitrile, gathers
One or more in lactic acid, Kynoar, polyvinyl alcohol, polymethyl methacrylate；
The mass fraction of CNT is 3-20% in the spinning solution, and the mass fraction of high molecular polymer is
2%-10%.
5. preparation method according to claim 3, it is characterised in that：The solvent N, N- dimethyl methyls
One or two or more kinds in acid amides, absolute ethyl alcohol, tetrahydrofuran, dichloromethane.
6. the CNT self-assembled nanometer fibrofelt described in a kind of claim 1 or 2 is in all-vanadium flow battery
In application, it is characterised in that：The CNT self-assembled nanometer fibrofelt is applied to as electrode material
In all-vanadium flow battery.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107677711A (en) * | 2017-10-30 | 2018-02-09 | 上海应用技术大学 | A kind of macromolecule liquid-sensitive sensor based on nano-graphene and preparation method thereof |
| CN111354952A (en) * | 2020-03-11 | 2020-06-30 | 沈阳建筑大学 | Graphite felt composite electrode and preparation method thereof |
| CN114212773A (en) * | 2021-12-17 | 2022-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of carbon nanotube film |
| CN116014080A (en) * | 2022-12-23 | 2023-04-25 | 成都先进金属材料产业技术研究院股份有限公司 | Titanium compound composite nano film and preparation method and application thereof |
| CN116377604A (en) * | 2022-12-23 | 2023-07-04 | 成都先进金属材料产业技术研究院股份有限公司 | Titanium carbide nano film and preparation method and application thereof |
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| CN104319409A (en) * | 2014-10-15 | 2015-01-28 | 中国科学院金属研究所 | High-activity asymmetric electrode for all-vanadium redox flow battery and preparation method thereof |
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| CN102713039A (en) * | 2010-01-21 | 2012-10-03 | 平松产业株式会社 | Carbon fiber nonwoven fabric, carbon fibers, method for producing the carbon fiber nonwoven fabric, method for producing carbon fibers, electrode, battery, and filter |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107677711A (en) * | 2017-10-30 | 2018-02-09 | 上海应用技术大学 | A kind of macromolecule liquid-sensitive sensor based on nano-graphene and preparation method thereof |
| CN111354952A (en) * | 2020-03-11 | 2020-06-30 | 沈阳建筑大学 | Graphite felt composite electrode and preparation method thereof |
| CN114212773A (en) * | 2021-12-17 | 2022-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of carbon nanotube film |
| CN116014080A (en) * | 2022-12-23 | 2023-04-25 | 成都先进金属材料产业技术研究院股份有限公司 | Titanium compound composite nano film and preparation method and application thereof |
| CN116377604A (en) * | 2022-12-23 | 2023-07-04 | 成都先进金属材料产业技术研究院股份有限公司 | Titanium carbide nano film and preparation method and application thereof |
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Application publication date: 20170620 |