CN102477693A - Activation method of carbon fiber electrode material using polyacrylonitrile carbon fiber - Google Patents
Activation method of carbon fiber electrode material using polyacrylonitrile carbon fiber Download PDFInfo
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- CN102477693A CN102477693A CN2010105547774A CN201010554777A CN102477693A CN 102477693 A CN102477693 A CN 102477693A CN 2010105547774 A CN2010105547774 A CN 2010105547774A CN 201010554777 A CN201010554777 A CN 201010554777A CN 102477693 A CN102477693 A CN 102477693A
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- carbon fiber
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Abstract
The invention belongs to an activation method of a carbon fiber electrode material. The invention adopts polypropylene carbon fiber weaved cloth soaked with epoxy resin as a raw material, and comprises the following steps of injecting air in a short time at a low vacuum condition with a temperature 600-700 DEG C, then performing vacuumization and natural cooling; thereby the surface properties of the carbon fiber cloth are improved, and the electrode activity is increased by more than 3 times.
Description
Technical field
The invention belongs to the activation method of carbon fibre electrode material that adopts polyacrylonitrile carbon fiber.
Background technology
Carbon fiber product has good corrosion resistance, electric conductivity, porous etc. a series of useful,
Physics, chemical property.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 treatments 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 l982 CR-167921 report it is the optimum condition of improving the chromium negative reaction that the viscose glue felt of l680 ℃ of carbonization supports gold one plumbous catalyst.Some companies of Japan do not adopt noble metal catalyst; Main research approach be higher temperature " l600-2500 ℃) under carry out carbonization after; In containing the oxygen inert atmosphere, carry out activation processing again. like twist flax fibers and weave 60263.164 open special permissions of company of Japan, containing through the cellulose carbon cloth of l600 ℃ of carbonization in the inert atmosphere of 200 torr oxygen, 850 ℃ handled 30 minutes.The oxygen atom of carbon fiber surface is than being increased to l0.2% from 2.5%, and the electrode electricity conductance 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.
Summary of the invention
The objective of the invention is to overcome above-mentioned technical problem, a kind of activation method of carbon fibre electrode material that adopts polyacrylonitrile carbon fiber is provided.
The present invention adopts industry to go up the polyacrylonitrile carbon fiber of about l300 ℃ carbonization, through removing part epoxy, in 60-0mmHg low vacuum condition, heats emptying, finds time, controls temperature again in (600-700) ± 60 ℃.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 industry to go up the polyacrylonitrile carbon fiber of about l300 ℃ carbonization, and the carbon fiber woven cloth in being no more than the epoxy resin acetone soln of 0.5% concentration after l-5 minute impregnation process is heated to 600 ~ 50 ℃ under 60-OmmHg low vacuum condition; After putting into 300mmHG～lat air; Find time, 8-l0 time repeatedly, range of temperature is (600-700) ± 50 ℃ again; Through 20 ~ 4O minute; Naturally cooling cooling, the carbon fiber table and epoxy resin carbonization after treatment, form the small porous body of three-dimensional structure. specific surface increases l and doubly increases with the upper surface oxy radical.
Electrode activity is carried merchant's result such as accompanying drawing l.Fig. 1 is 1cm
2Apparent electrode area exists
0.05mol/L in CrCl3～0.05mol/L FeCl2-1mol/L HCL electrolyte, 25 ℃,
0～0.95V (vs.SEC) potential range.Cyclic voltammetric characteristic (a) figure that is surveyed under the 10mv/S sweep speed is the measurement result of undressed carbon cloth electrode, and (b) figure is the measurement result of the heat treatment carbon cloth electrode of the inventive method.Contrast (a) is Cr on the curve (b)
3+/ Cr
2+And Fe
2+/ Fe
3+The right mixed oxidization reduction peak current of electricity can know that 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 following:
EXAMPLE l:
The polyacrylonitrile carbon fiber of about l300 ℃ carbonization in the industry is being no more than 0.6% concentration
Carbon fiber woven cloth in the cyclocyanide resin acetone soln after 1-5 minute impregnation process is warming up to 630 ℃ under 60-0mmHg low vacuum condition, put into l atm air; Find time, l0 time repeatedly, temperature natural fluctuates in 63O-780'C again; Through 40 minutes, cooling was cooled off naturally approximately.The surface nature of carbon fiber is improved after treatment, like the Table I data.Electrode activity improves
More than 3 times, like figure l.
Embodiment 2:
The polyacrylonitrile carbon fiber of about l300 ℃ carbonization in the industry, the carbon fiber woven cloth in being no more than the cyclochloride resin acetone soln of 0.5% concentration after 1-5 minute impregnation process is warming up to 600 ℃ under 60-0mmHg low vacuum condition; Put into the 300-400mmHg air; Find time, 8 times repeatedly, temperature natural fluctuates in 600-714 ℃ again; 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, like figure l.
Embodiment 3:
The polyacrylonitrile carbon fiber of about 1300 ℃ of carbonizations in the industry; Carbon fiber woven cloth in being no more than the epoxy resin acetone soln of 0.5% concentration after soaking the achievement processing in l-5 minute is under 60-0 mmHg low vacuum condition; Be warming up to 660 ℃ and put into 300-500 mmHg air, find time 8 times repeatedly again, temperature natural fluctuates in 550-680 ℃; Through 20 minutes, cooling was cooled off naturally approximately.After treatment carbon fiber surface character is improved, and electrode activity improves 3 times with as figure l.
Claims (2)
1. adopt the activation method of carbon fibre electrode material of polyacrylonitrile carbon fiber, it is characterized in that adopting industry to go up the polyacrylonitrile carbon fiber of about l300 ℃ carbonization.
2. the activation method of carbon fibre electrode material of employing polyacrylonitrile carbon fiber according to claim 1; Carbon fiber woven cloth in being no more than the epoxy resin acetone soln of 0.6% concentration after 1-5 minute impregnation process is that raw material is heated to 6 00 ± 60 ℃ under 60-0mmHg low vacuum condition, put into 300mmHg-latm air after, vacuumize again; 8-l is 0 time repeatedly; Variations in temperature is (600 1 700) ± 60 ℃, through 20-1 0 minute, and cooling cooling naturally.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105547774A CN102477693A (en) | 2010-11-23 | 2010-11-23 | Activation method of carbon fiber electrode material using polyacrylonitrile carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2010105547774A CN102477693A (en) | 2010-11-23 | 2010-11-23 | Activation method of carbon fiber electrode material using polyacrylonitrile carbon fiber |
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| CN102477693A true CN102477693A (en) | 2012-05-30 |
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| CN2010105547774A Pending CN102477693A (en) | 2010-11-23 | 2010-11-23 | Activation method of carbon fiber electrode material using polyacrylonitrile carbon fiber |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103334295A (en) * | 2013-06-07 | 2013-10-02 | 江苏大学 | Activation method for enhancing specific capacitance of polyacrylonitrile-based carbon fibers |
| CN105780364A (en) * | 2016-02-26 | 2016-07-20 | 浙江大学 | Method for preparing super-microporous flexible carbon cloth and product thereof and application |
| CN109671953A (en) * | 2017-10-13 | 2019-04-23 | 中国科学院大连化学物理研究所 | A kind of electrode material for all-vanadium flow battery and its preparation and application |
| CN109841851A (en) * | 2017-11-27 | 2019-06-04 | 中国科学院大连化学物理研究所 | A kind of electrode material for all-vanadium flow battery and its preparation and application |
-
2010
- 2010-11-23 CN CN2010105547774A patent/CN102477693A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103334295A (en) * | 2013-06-07 | 2013-10-02 | 江苏大学 | Activation method for enhancing specific capacitance of polyacrylonitrile-based carbon fibers |
| CN103334295B (en) * | 2013-06-07 | 2015-08-26 | 江苏大学 | A kind of activation method improving polyacrylonitrile-based carbon fibre ratio capacitance |
| CN105780364A (en) * | 2016-02-26 | 2016-07-20 | 浙江大学 | Method for preparing super-microporous flexible carbon cloth and product thereof and application |
| CN109671953A (en) * | 2017-10-13 | 2019-04-23 | 中国科学院大连化学物理研究所 | A kind of electrode material for all-vanadium flow battery and its preparation and application |
| CN109841851A (en) * | 2017-11-27 | 2019-06-04 | 中国科学院大连化学物理研究所 | A kind of electrode material for all-vanadium flow battery and its preparation and application |
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Application publication date: 20120530 |