CN1098560A - Activation method of carbon fibre electrode material - Google Patents

Activation method of carbon fibre electrode material Download PDF

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Publication number
CN1098560A
CN1098560A CN93109474A CN93109474A CN1098560A CN 1098560 A CN1098560 A CN 1098560A CN 93109474 A CN93109474 A CN 93109474A CN 93109474 A CN93109474 A CN 93109474A CN 1098560 A CN1098560 A CN 1098560A
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China
Prior art keywords
carbon fiber
activation method
electrode material
carbon
carbon fibre
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Pending
Application number
CN93109474A
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Chinese (zh)
Inventor
林兆勤
单义斌
江志韫
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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Priority to CN93109474A priority Critical patent/CN1098560A/en
Publication of CN1098560A publication Critical patent/CN1098560A/en
Pending legal-status Critical Current

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/96Carbon-based electrodes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/50Fuel cells

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inert Electrodes (AREA)

Abstract

The invention belongs to activation method of carbon fibre electrode material.
The present invention is a raw material with the polypropylene carbon fiber woven cloth of epoxy resin-impregnated, and under the low vacuum condition, the 600-700 ℃ following short time is put into air, finds time again, and natural cooling improves the carbon cloth surface nature, and electrode activity improves more than 3 times.

Description

Activation method of carbon fibre electrode material
The invention belongs to activation method of carbon fibre electrode material.
Carbon fiber product has a series of useful physical, chemical property such as good corrosion resistance, conductivity, porousness.Can be used for all kinds battery as electrode or auxiliary material, be one of stock of development novel energy storage cell.
But the electro-chemical activity of undressed carbon fiber is limited, and the chromium negative reaction of siderochrome redox flow flow pattern battery is for example only supporting noble metal catalysts such as gold or after special processings such as high temperature, carbon fiber just has electrode activity.
Different carbon fiber felts, different carburizing temperature, chemical cleaning method processing were once studied by the U.S., and factors such as different catalyst system and catalyzings are to the influence of carbon fiber felt electrode activity.Giner company thinks that in the NASA of nineteen eighty-two CR-167921 report it is the optimum condition of improving the chromium negative reaction that the viscose glue felt of 1630 ℃ of carbonizations supports gold-plumbous catalyst.
Some companies of Japan do not adopt noble metal catalyst, and mainly research approach is after carrying out carbonization under the higher temperature (1600~2500 ℃), carries out activation processing in containing oxygen natural instincts atmosphere again.As twist flax fibers and weave 60253.164 open special permissions of company of Japan, containing through the cellulose carbon cloth of 1600 ℃ of carbonizations in the inert atmosphere of 200 torr oxygen, 850 ℃ handled 30 minutes.The oxygen atom of carbon fiber surface is than being increased to 10.2% from 2.5%, and the electrode conductance rate improves, and the current efficiency of battery brings up to 96% from 90%.
Above carbon fiber preparation all needs high-temperature service, but also needs further activation processing.
The objective of the invention is to adopt the polyacrylonitrile carbon fiber of industrial about 1300 ℃ of carbonizations, through removing part epoxy, in 60~0mmHg low vacuum condition, heating emptying, find time, control temperature again in (600~700) ± 50 ℃, the carbon fiber that obtains at last, surface activity increases, and electrode reaction speed is accelerated greatly.
Characteristics of the present invention are to adopt the polyacrylonitrile carbon fiber of industrial about 1300 ℃ of carbonizations, carbon fiber woven cloth in being no more than the epoxy resin acetone soln of 0.5% concentration after 1~5 minute impregnation process, under 60~0mmllg low vacuum condition, be heated to 600 ± 50 ℃, after putting into 300mmllg~1atm air, find time, 8~10 times repeatedly, range of temperature is (600~700) ± 50 ℃ again, through 20~40 minutes, cooling cooling naturally.The carbonization after treatment of the epoxy resin of carbon fiber surface, the small porous body of formation three-dimensional structure.Specific surface increases more than 1 times, and surperficial oxy radical increases, and improve the wetability of the aqueous solution on the surface.The variation such as the table 1 of carbon fiber surface character before and after the heat treatment.
Carbon fiber surface character contrast before and after table 1 heat treatment
The surface group relative amount Before the heat treatment After the heat treatment
Electron spectroscopy analysis COOH C=0 or C-OH C 5.38 17.70 76.92 8.33 19.91 71.76
Specific surface (m 2/g) 133 320.2
Result such as accompanying drawing 1 that electrode activity improves.Fig. 1 is 1cm 2Apparent electrode area is at 0.05mol/L CrCl 3-0.05mol/L FeCl 2In-1mol/L HCl the electrolyte, at 25 ℃, 0-0.95vlvs.SCE) cyclic voltammetric characteristic (a) figure that surveyed under the potential range, 10mv/S sweep speed is the measurement result of undressed carbon cloth electrode, (b) figure is the measurement result of the heat treatment carbon cloth electrode of the inventive method.Cr on the contrast (a) and (b) curve 3+/ Cr 2+And Fe 2+/ Fe 3+The right mixed oxidization reduction peak current of electricity as can be known, than high more than 3 times before the heat treatment, institute's curve shape of surveying is stablized after the heat treatment, repeatedly sample in measurement result repetition.The heat treatment that the inventive method is described makes the carbon fiber surface activation, and electrode reaction speed is accelerated greatly.
Carbon cloth poling processing technique embodiment provided by the invention is as follows:
Embodiment 1:
The polyacrylonitrile carbon fiber of industrial about 1300 ℃ of carbonizations, carbon fiber woven cloth in being no more than the epoxy resin acetone soln of 0.5% concentration after 1~5 minute impregnation process, under 60~0mmHg low vacuum condition, be warming up to 630 ℃, put into the 1atm air, find time again, 10 times repeatedly, the fluctuation in 630~730 ℃ of temperature nature, through 40 minutes, cooling was cooled off naturally approximately.The surface nature of carbon fiber is improved after treatment, as table 1 data.Electrode activity improves more than 3 times, as Fig. 1.
Embodiment 2:
The polyacrylonitrile carbon fiber of industrial about 1300 ℃ of carbonizations, carbon fiber woven cloth in being no more than the epoxy resin acetone soln of 0.5% concentration after 1~5 minute impregnation process, under 60~0mmHg low vacuum condition, be warming up to 600 ℃, put into 300~400mmHg air, find time again, 8 times repeatedly, the fluctuation in 600~714 ℃ of temperature nature, through 30 minutes, cooling was cooled off naturally approximately.Carbon fiber surface character is after treatment improved, and electrode activity improves more than 3 times, as Fig. 1.
Embodiment 3:
The polyacrylonitrile carbon fiber of industrial about 1300 ℃ of carbonizations, carbon fiber woven cloth in being no more than the epoxy resin acetone soln of 0.5% concentration after soaking the achievement processing in 1~5 minute, under 60~0mmHg low vacuum condition, be warming up to 550 ℃ and put into 300~500mmHg air, find time again, 8 times repeatedly, the fluctuation in 550~680 ℃ of temperature nature, through 20 minutes, cooling was cooled off naturally approximately.Carbon fiber surface character is after treatment improved, and electrode activity improves more than 3 times, as Fig. 1.

Claims (1)

1, a kind of activation method of carbon fibre electrode material, it is characterized in that adopting the polyacrylonitrile carbon fiber of industrial about 1300 ℃ of carbonizations, carbon fiber woven cloth in being no more than the epoxy resin acetone soln of 0.5% concentration after 1-5 minute impregnation process is that raw material is heated to 600 ± 50 ℃ under 60~0mmHg low vacuum condition, after putting into the 300mmHg-1atm air, vacuumize, 8-10 time repeatedly, variations in temperature is (600~700) ± 50 ℃ again, through 20-40 minute, cooling cooling naturally.
CN93109474A 1993-08-03 1993-08-03 Activation method of carbon fibre electrode material Pending CN1098560A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN93109474A CN1098560A (en) 1993-08-03 1993-08-03 Activation method of carbon fibre electrode material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN93109474A CN1098560A (en) 1993-08-03 1993-08-03 Activation method of carbon fibre electrode material

Publications (1)

Publication Number Publication Date
CN1098560A true CN1098560A (en) 1995-02-08

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Application Number Title Priority Date Filing Date
CN93109474A Pending CN1098560A (en) 1993-08-03 1993-08-03 Activation method of carbon fibre electrode material

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CN (1) CN1098560A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1066215C (en) * 1998-06-20 2001-05-23 中山大学 Extraction of metal silver by modified active carbon fiber reduction adsorption
CN101597862B (en) * 2009-06-18 2012-08-22 天华溢威特种纤维(新泰)有限公司 Method for improving carbon fiber surface activity
CN107934955A (en) * 2017-11-17 2018-04-20 浙江大学 A kind of method of activation process commercialization carbon cloth

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1066215C (en) * 1998-06-20 2001-05-23 中山大学 Extraction of metal silver by modified active carbon fiber reduction adsorption
CN101597862B (en) * 2009-06-18 2012-08-22 天华溢威特种纤维(新泰)有限公司 Method for improving carbon fiber surface activity
CN107934955A (en) * 2017-11-17 2018-04-20 浙江大学 A kind of method of activation process commercialization carbon cloth

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