CN105869927A - Method for preparing high-specific-surface-area and high-specific-capacitance carbon fibers by random copolymers - Google Patents

Method for preparing high-specific-surface-area and high-specific-capacitance carbon fibers by random copolymers Download PDF

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CN105869927A
CN105869927A CN201610479220.6A CN201610479220A CN105869927A CN 105869927 A CN105869927 A CN 105869927A CN 201610479220 A CN201610479220 A CN 201610479220A CN 105869927 A CN105869927 A CN 105869927A
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carbon fiber
specific
acrylonitrile
temperature
carbon fibers
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CN105869927B (en
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薛怀国
徐浩
宋欣
徐梦娇
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Yangzhou University
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Yangzhou University
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    • 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
    • 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
    • H01G11/32—Carbon-based
    • H01G11/40—Fibres
    • 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 belongs to the technical field of sustainable energy sources and discloses a method for preparing high-specific-surface-area and high-specific-capacitance carbon fibers by random copolymers. The method includes: dissolving acrylonitrile acrylate copolymer into N,N- dimethyl formamide to obtain a spinning solution, using the spinning solution for preparing acrylonitrile-acrylate copolymer nanofibers according to an electrospinning method, and performing pre-oxidization and carbonization to obtain polyacrylonitrile-based copolymer carbon fibers; mixing the polyacrylonitrile-based copolymer carbon fibers with KOH aqueous solution, and activating to obtain the high-specific-surface-area and high-specific-capacitance carbon fibers. The method has advantages of technical simplicity, adjustability of spinning fibers, environment friendliness and the like. A supercapacitor is an energy storage element between a traditional capacitor and a battery and has advantages of high power density, high energy density, quickness in charging and discharging and long cycle life.

Description

A kind of random copolymer prepares high-specific surface area and the method for high specific capacitance carbon fiber
Technical field
The invention belongs to sustainable energy technology, be specifically related to the production technical field of ultracapacitor.
Background technology
Electrostatic spinning technique be a kind of can rapidly, continuously, simple and effective acquisition nanometer to the method for several micron order fibers.The features such as spinning fibre has that technique is simple, fibre diameter is adjustable, high-specific surface area and porosity.Therefore the fields such as bioengineered tissue, gas-liquid filtration, sensing material it are widely used in.During electrostatic spinning, polymer solution or melt charge accumulated under the effect of high voltage electric field, electric field tensile force gradually exceedes the surface tension of polymeric liquid, and polymer solution sprays, stretches and along with solvent volatilization or melt cooling are gradually solidified into silk, receiving terminal acquisition nanofiber.
Ultracapacitor, is again electrochemical capacitor, stores energy by adion or quickly surface oxidation reduction reaction.The fields such as ultracapacitor, as a kind of Novel energy storage apparatus, has power density high, has extended cycle life, and charge/discharge rates is fast and the advantage such as environmental protection, is widely used in information technology, electric automobile, space flight and aviation, science and techniques of defence.According to the difference of its energy storage mechnism, double layer capacitor can be divided into, Faraday pseudo-capacitance itself and hybrid capacitors three kinds.Double layer capacitor mainly carrys out energy storage by the electric double layer capacitance formed on electric charge interface between electrode and electrolyte.The electrode material of double layer capacitor is usually porous charcoal, and by the diffusion of electrolyte, ion forms electric double layer in the duct of electrode material, and therefore the ratio electric capacity of double layer capacitor depends on specific surface and the pore structure of electrode material.Faraday pseudo-capacitance device is mainly by carrying out energy storage in the surface of electrode material or the redox reaction of near surface generation Rapid reversible or chemisorbed/desorption, the feature of this reaction is that the transfer of electric charge occurs on the surface of electrode or near surface and has the faradic currents of non-continuous to produce, its electrode material is mainly metal oxide, conducting polymer etc..Hybrid capacitors has two kinds of energy storage mechnism concurrently, and two electrodes are made up of fake capacitance class or battery class electrode material and porous charcoal respectively.
Prior art prepares the defect that high specific capacitance carbon fiber exists: carbon fiber is a kind of in fibrous activated carbon material, mainly by precursor fibre is carried out low temperature pre-oxidation, then obtains in conjunction with high temperature cabonization.At present, preparing carbon fiber and be primarily present two problems: 1, under carburizing temperature, the linear copolymer structure assembled is unstable；2, the carbon productivity of most of copolymers is relatively low.
Summary of the invention
The defect existed for above prior art, the present invention seeks to propose a kind of random copolymer and prepares high-specific surface area and the method for high specific capacitance carbon fiber.
The present invention comprises the following steps:
1) acrylonitrile acrylic copolymer P(AN-co-AA is formed by radical polymerization), by acrylonitrile acrylic copolymer P(AN-co-AA) be dissolved in DMF, form spinning solution；Acrylonitrile-acrylic acid copolymer nanofiber is made by electrospinning process；
2) use tube furnace acrylonitrile-acrylic acid copolymer nanofiber is pre-oxidized successively, carbonization treatment, obtain polyacrylonitrile base co-polymer carbon fiber；
3) polyacrylonitrile base co-polymer carbon fiber is mixed post activation with the KOH aqueous solution, obtain high-specific surface area and high specific capacitance carbon fiber.
The present invention passes through radical polymerization synthesis of acrylonitrile acrylic copolymer, by electrostatic spinning technique, with DMF as solvent, is prepared for acrylonitrile-acrylic acid copolymer nanofiber.Research shows: the addition of a small amount of acrylic acid copolymer component can improve morphology of carbon fibers, but the most acrylic acid add membership and cause carbon fiber to shrink aggravation, has bead string phenomenon to produce；The increase of copolymerization component ratio can increase the degree of roughness of fiber surface, and plays certain reaming effect.
Then utilize tube furnace that electrospinning fibre is carried out carbonization treatment, obtain polyacrylonitrile base co-polymer carbon fiber, and by ESEM and absorption test, carbon fiber is characterized, result shows that the addition of acrylate makes carbon fiber have certain contraction, and along with the increase of acrylic acid content, shrink even more serious, fiber morphology heterogeneity.
By the carbon fiber obtained with KOH mixing activate, activation process be activator with carrying out the process of complex chemical reaction between material with carbon element, can be with the specific surface area of controlled material, pore-size distribution and surface heteroatom group.The material with carbon element of high-specific surface area is ultimately formed by run-inflation effect, dehydration, fragrance condensation and skeleton function.Carbon fiber activation obtained carries out electro-chemical test, and result shows effectively to obtain the electrode material of high specific capacitance, as the application of ultracapacitor.
It is simple that the inventive method has technique, the advantages such as spinning fibre is adjustable, environmental protection.Spinning fibre size average 150～200 Nm, carbon fiber specific surface area 2117 m2·g-1, the ratio electric capacity of ultracapacitor is up to 300 F ·g-1.This ultracapacitor is a kind of energy-storage travelling wave tube between traditional capacitor and battery, has power density big, the advantage that energy density is high, and charge/discharge rates is fast, has extended cycle life, environmentally safe.
Further, acrylonitrile acrylic copolymer P(AN-co-AA of the present invention) it is 1: 9 with the mixing quality ratio of DMF.With this spinning solution formed, there is suitable viscosity, in order to spinning goes out size uniform smoothly, does not has the spinning fibre of beading.
During described electrostatic spinning, voltage is 16 kV, and the flow velocity of spinning solution is 0.1 mm/min, and the distance between spinneret and receiver is 14 cm.Spinning fibre size uniformity can be obtained, it is ensured that the fiber made does not has bead string phenomenon.
The temperature of described pre-oxidation, time conditions are 200～300 DEG C, 120min.The temperature time protocols of preferred described pre-oxidation is 240 DEG C.When temperature is 240 DEG C, P(AN-co-AA) morphology of carbon fibers structure is the most stable.
The temperature of described carbonization, time conditions are 700～900 DEG C, 120min.The carbon fiber that under this temperature range, carbonization obtains has certain nitrogen content, and has certain degree of graphitization.The temperature of preferred described carbonization is 800 DEG C, and the electrode material chemical property that the carbon fiber obtained does ultracapacitor is best.
Described polyacrylonitrile base co-polymer carbon fiber is 1: 4 with the mixing quality ratio of KOH.Under the conditions of Gai, activation effect be best, obtains big specific surface area, wide pore-size distribution carbon fiber.
The temperature conditions of described activation is 700～900 DEG C.Activating under this temperature range, carbon fiber has certain nitrogen content, and has certain degree of graphitization.
Further, the temperature conditions of described activation is 800 DEG C, activates at such a temperature, is ultimately formed the carbon fiber of high-specific surface area by run-inflation effect, dehydration and skeleton function.
Accompanying drawing explanation
Fig. 1 is the SEM Electronic Speculum figure of the fiber using electrospinning process to be formed.
Fig. 2 is P(AN-co-AA) PAN-ACF desorption curve.
Fig. 3 is three-electrode system carbon fiber cyclic voltammogram.
Fig. 4 is three-electrode system carbon fiber constant current charge-discharge curve map.
Detailed description of the invention
1, spinning fibre is prepared:
12.1g acrylonitrile, 1.34g acrylic acid, 47.3g dimethyl sulfoxide (DMSO) are added there-necked flask, add 0.61g azodiisobutyronitrile (AIBN), be sufficiently stirred for and lead to nitrogen 20 min, being heated to 60 DEG C, react 12 h, prepare acrylonitrile acrylic copolymer P(AN-co-AA).
Take 0.6g acrylonitrile acrylic copolymer P(AN-co-AA) it is dissolved in 5.4g DMF solvent, it is sufficiently stirred for 12 h, obtains the spinning solution of mass fraction 10%.
Electrostatic spinning operates: draws appropriate spinning solution with syringe, and loads onto spinning syringe needle on its top, is connected with positive source.Receive with aluminium foil, be connected with receiving plate as negative pole.The flow velocity of the spinning solution i.e. fltting speed of syringe is by micro-injection pump control, until syringe needle has stable droplet to occur, applies high pressure, and controlling voltage is 16 KV, flow velocity is 0.1 Mm/min, the distance between spinneret and receiver is 14cm, i.e. can get continuous print acrylonitrile-acrylic acid copolymer nanofiber, as it is shown in figure 1, spinning fibre size uniformity, it is ensured that the fiber made does not has bead string phenomenon.
2, polyacrylonitrile base co-polymer carbon fiber is prepared:
The preparation process of polyacrylonitrile base co-polymer carbon fiber is to carry out in temperature automatically controlled tube furnace, including pre-oxidation and two stages of carbonization.
The corundum boat that will be equipped with acrylonitrile-acrylic acid copolymer nanofiber is placed in tube furnace center, quartz ampoule two ends are kept to communicate with air, heating rate is 1.5 DEG C/min, it is warming up to 240 DEG C of insulations and carries out pre-oxidation treatment 120min, seal tube furnace subsequently, in a nitrogen atmosphere, be warming up to 800 DEG C with 5 DEG C/min and carry out carbonization treatment 120min, automatically it is cooled to room temperature, i.e. obtains polyacrylonitrile base co-polymer carbon fiber.
3, high-specific surface area and high specific capacitance carbon fiber (i.e. activating process) are prepared:
Polyacrylonitrile base co-polymer carbon fiber after 0.2g carbonization is mixed with 0.8g KOH, adds 20mL water uniform stirring.Gained mixture is dried in 110 DEG C of baking ovens 12 H, is placed in dried mixture in tube furnace, under nitrogen air-flow protection, and 5 DEG C/min of programming rate, it is warming up to 800 DEG C of constant temperature 60 min of activation temperature, room temperature is down to by tube furnace subsequently.By products therefrom with 1 The HCl/water solution of M washes away alkaline matter, then is washed with deionized water to neutrality, is finally placed in 110 DEG C baking oven in be dried 24 H, obtains high-specific surface area and high specific capacitance carbon fiber after cooling.
When 77K, carbon fiber is carried out nitrogen adsorption desorption test as in figure 2 it is shown, as seen from Figure 2: during electrostatic spinning, acrylonitrile section is thrown away with acrylic acid section and mixed mutually, and when carbonization, acrylic acid section carboxyl is pyrolyzed pore-forming.
4, high-specific surface area and each performance verification of high specific capacitance carbon fiber:
Weigh high-specific surface area that above method of the present invention made by the ratio that mass ratio is 8:1:1 and high specific capacitance carbon fiber is put in little mortar with conductive agent acetylene black, adhesive polytetrafluoroethylene (PTFE), dropping isopropanol, constantly grind and dropwise drip isopropanol, being mixed by mixture, drop coating is in the nickel foam of 1*5 cm.The nickel sheet that drop coating is good is placed in 80 DEG C dry 6 hours in vacuum drying oven, is pressed into smooth thin slice (pressure 10 MPa), is dried 12 hours with 120 DEG C after being cooled to room temperature.The foam nickel electrode prepared, mercury/mercuric oxide electrode and platinum plate electrode are placed in KOH electrolyte and constitute three electrode work systems, wherein foam nickel electrode is working electrode, mercury/mercuric oxide electrode is reference electrode, platinum plate electrode is to electrode, electrochemical workstation is used to be circulated volt-ampere, obtaining figure as shown in Figure 3, constant current charge-discharge is tested as shown in Figure 4.
In Fig. 3, curve A to E represents the cyclic voltammetry curve obtained under the sweep speed of 5,10,20,50,100 mv/s respectively, and electrode material all can keep approximate rectangular topography profile, shows that material has good high rate performance under sweeping greatly speed.
Fig. 4, A to E represents the constant current charge-discharge curve obtained under the current density of 10,5,2,1,0.6 A/g respectively, different current density lower curves all keep approximating isosceles triangle feature, even if illustrative material is maintained to preferable capacitive characteristics under big current density.

Claims (10)

1. a random copolymer prepares high-specific surface area and the method for high specific capacitance carbon fiber, it is characterised in that comprise the following steps:
1) form acrylonitrile acrylic copolymer by radical polymerization, acrylonitrile acrylic copolymer P is dissolved in DMF, form spinning solution；Acrylonitrile-acrylic acid copolymer nanofiber is made by electrospinning process；
2) use tube furnace acrylonitrile-acrylic acid copolymer nanofiber is pre-oxidized successively, carbonization treatment, obtain polyacrylonitrile base co-polymer carbon fiber；
3) polyacrylonitrile base co-polymer carbon fiber is mixed post activation with the KOH aqueous solution, obtain high-specific surface area and high specific capacitance carbon fiber.
Method the most according to claim 1, it is characterised in that: described acrylonitrile acrylic copolymer P is 1: 9 with the mixing quality ratio of DMF.
Method the most according to claim 1, it is characterised in that: during described electrostatic spinning, voltage is 16 kV, and the flow velocity of spinning solution is 0.1 mm/min, and the distance between spinneret and receiver is 14 cm。
Method the most according to claim 1, it is characterised in that: the temperature of described pre-oxidation is 200～300 DEG C, and the time is 120min.
Method the most according to claim 4, it is characterised in that: the temperature of described pre-oxidation is 240 DEG C.
6. according to the method described in claim 1 or 4 or 5, it is characterised in that: the temperature of described carbonization is 700～900 DEG C, and the time is 120min.
Method the most according to claim 6, it is characterised in that: the temperature of described carbonization is 800 DEG C.
Method the most according to claim 1, it is characterised in that: described polyacrylonitrile base co-polymer carbon fiber is 1: 4 with the mixing quality ratio of KOH.
Method the most according to claim 1, it is characterised in that: the temperature conditions of described activation is 700～900 DEG C.
Method the most according to claim 9, it is characterised in that: the temperature conditions of described activation is 800 DEG C.
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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN110485001A (en) * 2019-08-05 2019-11-22 武汉纺织大学 A method of activated carbon fiber is prepared based on centrifugal spinning
CN114351293A (en) * 2021-12-28 2022-04-15 吉林大学 Nano YAG (yttrium aluminum garnet) -doped polyacrylonitrile-based mesoporous activated carbon fiber and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110485001A (en) * 2019-08-05 2019-11-22 武汉纺织大学 A method of activated carbon fiber is prepared based on centrifugal spinning
CN114351293A (en) * 2021-12-28 2022-04-15 吉林大学 Nano YAG (yttrium aluminum garnet) -doped polyacrylonitrile-based mesoporous activated carbon fiber and preparation method thereof
CN114351293B (en) * 2021-12-28 2022-09-30 吉林大学 Nano YAG (yttrium aluminum garnet) -doped polyacrylonitrile-based mesoporous activated carbon fiber and preparation method thereof

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