CN1332082C - Graphitization preparation process for carbon fiber by using radio frequency method and production system thereof - Google Patents
Graphitization preparation process for carbon fiber by using radio frequency method and production system thereof Download PDFInfo
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- CN1332082C CN1332082C CNB2004100122397A CN200410012239A CN1332082C CN 1332082 C CN1332082 C CN 1332082C CN B2004100122397 A CNB2004100122397 A CN B2004100122397A CN 200410012239 A CN200410012239 A CN 200410012239A CN 1332082 C CN1332082 C CN 1332082C
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- carbon fiber
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- boron chloride
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Abstract
The present invention relates to a graphitization preparation process for carbon fibers by a radio frequency method and a preparation system thereof. The preparation process adopts the induction heating mode of a radio frequency method for finishing the graphitization conversion of carbon fibers; the complete process comprises carbon fiber degumming, boron trichloride infiltration, drying, radio frequency induction heating to 2400 DEG C to 3000 DEG C, the immersion of epoxy resin glue on the surface, and drying; the complete preparation process is finished under the differential speed tension of a filament collecting and releasing mechanism. Matched preparation systems comprise a filament releasing machine, a degumming furnace, a boron trichloride immersion trough, a drying tank, a high frequency heater, a glue immersion trough, a drying tank and a filament collecting machine which are orderly arranged to form a main apparatus; a flow control meter, a radio frequency generator, a power matching apparatus and a microcomputer regulation and control system form a process supporting apparatus.
Description
Technical field
The invention belongs to radio frequency method is realized the improvement of carbon fiber and graphite production technology and production system and perfect.
Background technology
The production technology of carbon fiber and graphiteization promptly is to be raw material when being heated to more than 2400 ℃ high temperature with the carbon fiber, makes the carbon molecule become the ordered lattice structure by lasting drafting force, thereby finishes by the conversion of common carbon molecule to the graphitization molecule.The inventor has initiated the process technology of radio frequency method, promptly by the RF high power generator, with the direct line focus of energy of electromagnetic field and be carried on the carbon fiber, finishes graphited conversion in special radio frequency thermal reactor.This processing technique equipment is simple, regulates and control easyly and accurate, has greatly saved the energy and reduced cost, is the once breakthrough improvement in this area, has solved the firing equipment and the good technique of most critical in the carbon fiber and graphite processing.In concrete continuous flow procedure, also must relate to the surface treatment of carbon fiber processing front and back, oxidation protection in the high-temperature process and further improve the intensity on graphitized carbon fibre surface and improve it and do the technical indicators such as surface affinity of composite, also to solve in the process treatment process quantity-produced stability under the hot environment etc., all need production technology and relevant production equipment done further and improve.
Summary of the invention
The object of the present invention is to provide a radio frequency method carbon fiber and graphite production technology and a production system thereof that is suitable for the serialization production requirement.
The present invention is on the basis of radio frequency method carbon fiber and graphite processing technology and special equipment, and production technology and production equipment system are further improved.The heating process of this production technology key is that the radio-frequency electromagnetic field energy is at first finished line focus by means of coaxial conjugation coupling cavity, make the carbon fiber quartz ampoule thermal reactor eddy-current heating to 2400 by deoxidation ℃～3000 ℃ continuously, and under constant force drawing-off state, finish graphited conversion process in the thermal treatment zone, be complete production technology of supporting formation, by repetition test, the inventor increases to following complete process process with design in the continuous processing technology again:
A. carbon fiber comes unstuck.As the raw material in this process, all handle at the front surface that dispatches from the factory through gluing, if this sizing material is not removed, in heating process, can at high temperature produce a large amount of pernicious gases, directly have influence on the processing and the quality of carbon fiber.
B. the carbon fiber after will coming unstuck soaks into boron chloride.Its effect is to infiltrate boron chloride in the carbon fiber before processing.Can under micro-hydrogen effect, be reduced into boron after entering quartz tube reactor be deposited on carbon fiber surface, thus the affinity when improving the surface strength of carbon fiber and Application of composite greatly.
C. oven dry.To soak the carbon fiber oven dry of boron chloride, so that boron chloride is attached to the carbon fiber surface layer.
D. under argon gas and micro-nitrogen environment, be heated to graphitization temperature.
E. gluing.At graphitized carbon fibre surface applied epoxide-resin glue.
F. oven dry.The resin glue oven dry is formed the glue finishing coat of graphitized carbon fibre.
Above operation is finished under the continuous differential traction of receiving the thread supplying machine system successively.
For finishing above operation, ad hoc to have counted supporting production system as follows:
1, the adjustable bull of differential is received thread supplying machine.This equipment is arranged on the two ends of production system, and the linear differential decision of setting with folding and unfolding silk wheel is applied to the drafting force on the continuous carbon fibre.
2, radio-frequency signal generator and supporting power match device, its produces radio frequency and can and be loaded on radio frequency conjugation coupling cavity and the supporting quartz tube reactor that is located in the coupling cavity is formed radio frequency heating apparatus jointly by matching relationship, and this heater is located in the middle of the differential folding and unfolding silk mechanism.
3, be located at and be provided with degumming stove necessary in the processes, boron chloride immersion trough and drying baker between thread supplying machine and the heater.
4, be located at heater and receive steeping vat between the silk machine, drying baker.
5, the gas flowmeter of decision process environments.
6, the microcomputer management system of monitoring and regulating and control by process conditions.
Carbon fiber to be processed is drawn from thread supplying machine.Pass the every special equipment of 1-5 by the middle directive wheel between the equipment of being located at, cause the cops of receiving the silk machine, again each technological parameter value initialization is stored in the memory of microcomputer, state with each equipment under the regulation and control of control system transfers to required process conditions, can enter full automatic graphitized carbon fibre production process.
The technology and the production system that further specify among the present invention below in conjunction with accompanying drawing are how to realize goal of the invention.
Description of drawings
Accompanying drawing 1 is that the radio frequency method carbon fiber and graphite technological process of production and production equipment system are formed schematic diagram.
Wherein 1 represent thread supplying machine, 2 represent degumming stove, and 3 represent the boron chloride immersion trough, and 4 represent drying baker, the heating generator that 5 representatives are made up of coaxial conjugation coupling cavity 5A and quartz tube reactor 5B.6 represent steeping vat, and 7 represent drying baker, and the silk machine is received in 8 representatives, and 9 represent gas flowmeter, and 10 represent radio-frequency signal generator, and 11 represent the adaptation of radio frequency power output, and 12 represent the microcomputer management system of whole process control parameters of contain and management software.
The specific embodiment
Accompanying drawing 1 is given is the structural representation of the production equipment system that provides by continuous production processes.Demonstrating among this figure with the continuous carbon fibre is raw material, and the carbon fiber and graphite metallization processes that is heated to be the graphitization heater means with radio frequency induction should comprise following complete technological.
A, carbon fiber is come unstuck: this operation is carried out in special equipment degumming stove 2, process conditions are that the physics under nitrogen environment comes unstuck, temperature in the stove is remained between 600 ℃-700 ℃, be full of nitrogen and form the deoxidation environment, can make the glue gasification and discharge with waste gas.
B, the back carbon fiber that will come unstuck soak into boron chloride: this operation is to finish in boron chloride immersion trough 3, and the carbon fiber after coming unstuck enters drying baker 4 successively by immersion trough behind the infiltration boron chloride, and the purity of boron chloride should be and is not less than 99.99%.
C, oven dry are finished in drying baker 4, and bake out temperature is 180 ℃-240 ℃, and the carbon fiber after the oven dry enters the quartz tube reactor 5B in the high frequency heat reactor 5.
D, in the anti-device 5B of radio frequency quartz ampoule heat, finish the conversion of carbon fiber and graphiteization, between 2400 ℃-3000 ℃ of the processed fiber temperatures.Concrete process conditions are: from filament inlet and the filament mouth two ends input protection gas argon gas of quartz ampoule thermal reactor 5B, wherein mix and mix a spot of arc extinguishing gases nitrogen 1-5%, wherein the remaining oxygen in the argon gas is less than 0.1ppm, and the residual water yield is less than 1ppm.The filament inlet end is imported micro-hydrogen when injecting protective gas and arc extinguishing gases nitrogen, charge into the 0.1-0.5% that amounts of hydrogen is an argon flow amount.
E, graphitized carbon fibre is entered steeping vat 6, successively by filling the glue groove of epoxide-resin glue.Also can apply different glue faces according to the difference of product final use.Fiber enters drying baker 7 behind the gluing.
F, oven dry: the drying baker environment temperature is between 180 ℃-240 ℃.
It is stand-by that finished fiber after the oven dry is wound in coil packing by a receipts silk machine.
Keeping the normal flow of gas argon gas in above operation is 1.0-2.0 liter/hour k silk, that is to say that the flow-control originally of protection gas is relevant with the radical of tow.The 1k silk is different with the 3k silk, and a synnema is different with the multi beam silk, can carry out accommodation as the case may be.
The average linear velocity of carbon fiber in processing quartz ampoule thermal reactor 5B is the 69m-132m/ branch, and wherein receiving the ratio that silk machine wrap wire speed and thread supplying machine put silk thread speed is 1.005-1.02: 1.
Accompanying drawing 1 is shown as to produce realizes this technological design and necessary production equipment system structural representation.
Wherein radio-frequency signal generator 10 and power match device 11 are energy resource supply isolated plants of graphitization processing, and it is core special equipments with coaxial conjugation coupling cavity 5A and the common heating generator of forming 5 of quartz ampoule thermal reactor 5B.Had detailed statement (visible patent 01100536.X) in the patent that the design people has applied for.In realizing the system that serialization is produced, also comprise the degumming stove 2 that is located between thread supplying machine 1 and the heating generator 5, boron chloride immersion trough 3, drying baker 4.And be located at heating generator 5 and receive coating groove 6 and drying baker 7 between the silk machine 8.More than device is sequentially arranged in by between the retractable silk machine (1,8), and carbon fiber is together in series successively and forms a main body production structure.By gas flowmeter 9, the auxiliary equipment system that provides technology to support is provided for radio-frequency signal generator 10 and power match device 11, under the monitoring of the microcomputer system of storage standard technology data and management software 12 and regulation and control, realize automatic continuous production, nitrogen, argon gas, hydrogen is respectively by gas flowmeter 9 technological equipment with normal flow input appointment under computer instruction, and the technological parameter collection of the equipment that arrives according to on-line monitoring input computer is as the foundation of regulation and control, constantly to gas flowmeter 9 and power match device 11 and receive thread supplying machines (1,8) and send regulation and control instruction and guarantee that whole processing technology finishes the continuous graphitization processed under the strict process condition.
For improving the whole system working (machining) efficiency, receiving silk machine 1 and thread supplying machine 8 can take the structure of 1-12 head to form the radio and tape player silk device that parallel type can independently be regulated and control, corresponding supporting be that the structure of heating generator 5 will be that (coupling cavity is flat in single chamber, referring to No. 02103976.3 patent application) and the quartzy hot anti-device 5B composition of 1-12 root, its corresponding process conditions are with the correspondence adjustment.
According to the carbon fiber and graphite production technology that this technology and equipment are determined, simplified the electric furnace process production process that still adopts in the world at present widely.Its simplified control, accurately fast, the energy is significantly saved the graphite fibre production cost is declined to a great extent in regulation and control, and the discreteness of product obviously reduces, and helps the promotion and application of new material.
Claims (10)
1, radio frequency method carbon fiber and graphite production technology, this process using RF linear focusing arrangement is heated to 2600-3000 ℃ with carbon fiber under the deoxidation environment, make carbon fiber under constant force drawing-off state, realize graphitization processing by the linear thermal treatment zone continuously, it is characterized in that this continuous production processes comprises following operation:
A, carbon fiber come unstuck
B, the carbon fiber that comes unstuck soak into boron chloride
C, oven dry
D, enter in the quartz ampoule thermal reactor (5B) and be heated to graphitization temperature
E, impregnation
F, oven dry.
2,, it is characterized in that the process conditions when heating carbon fiber temperature is 2600 ℃-3000 ℃ in quartz ampoule thermal reactor (5B) are according to the said carbon fiber and graphite production technology of claim 1:
1. the protective gas that injects from quartz ampoule radio frequency thermal reactor (5B) filament inlet, filament mouth two ends is an argon gas, remaining oxygen＜0.1ppm in the argon gas, and the residual water yield is less than 1ppm,
2. sneak into 1-5% arc extinguishing nitrogen in the protective gas,
3. go into argon gas that a thread port injects and also add the hydrogen of 0.1%-0.5%.
3,, it is characterized in that Degumming Procedures is to finish 600-700 ℃ of the temperature of coming unstuck in the degumming stove (2) at nitrogen atmosphere according to the said carbon fiber and graphite production technology of claim 1.
4, according to the said carbon fiber and graphite production technology of claim 1, it is characterized in that carbon fiber soak into boron chloride be by carbon fiber continuously by finishing in the boron chloride immersion trough (3), the purity of boron chloride is not less than 99.99%.
5,, it is characterized in that impregnation is to be finished by epoxide-resin glue groove (6) continuously by graphitized fibre according to the said carbon fiber and graphite production technology of claim 1.
6, according to the said carbon fiber and graphite production technology of claim 1, the bake out temperature of its feature after soaking boron chloride and epoxy resin dipping glue is 180-240 ℃.
7, according to the said carbon fiber and graphite production technology of claim 2, the flow that it is characterized in that the protective gas argon gas is 1.0-2.0 liter/hour K silk.
8, according to the said carbon fiber and graphite metallization processes of claim 1, it is characterized in that quartz ampoule thermal reactor (5B) average linear velocity that carbon fiber passes through is the 69-132m/ branch, receipts silk machine wrap wire speed is 1.005-1.02 with the ratio that thread supplying machine is put silk thread speed: 1.
9, radio frequency method carbon fiber and graphite production system, comprise radio-frequency signal generator (10), the coaxial conjugation coupling cavity (5A) of power match device (11) and line focus, and be located at quartz ampoule thermal reactor (5B) in the chamber, and supporting differential radio and tape player (1,8), it is characterized in that also being provided with in the native system degumming stove (2) that is provided with by the described process sequence of claim 1, boron chloride immersion trough (3), drying baker (4), steeping vat (6) and drying baker (7), gas flowmeter (9), and the Control System of Microcomputer of the monitoring of technological parameter and regulation and control (12).
10, according to the said carbon fiber and graphite production system of claim 9, it is characterized in that receiving thread supplying machine (1,8) being 1-12 the folding and unfolding silk device that controlled folding and unfolding silk machine is formed, is corresponding single chamber 1-12 pipe radio frequency thermal reaction apparatus in the supporting high frequency induction heater (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100122397A CN1332082C (en) | 2004-04-19 | 2004-04-19 | Graphitization preparation process for carbon fiber by using radio frequency method and production system thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100122397A CN1332082C (en) | 2004-04-19 | 2004-04-19 | Graphitization preparation process for carbon fiber by using radio frequency method and production system thereof |
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| CN1690261A CN1690261A (en) | 2005-11-02 |
| CN1332082C true CN1332082C (en) | 2007-08-15 |
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| CNB2004100122397A Expired - Fee Related CN1332082C (en) | 2004-04-19 | 2004-04-19 | Graphitization preparation process for carbon fiber by using radio frequency method and production system thereof |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101988222B (en) * | 2009-07-31 | 2013-11-13 | 王敬霞 | Radio-frequency heating carbon fiber graphitization continuous batching production system and method |
| CN104975512A (en) * | 2015-07-20 | 2015-10-14 | 深圳中飞腾翔航空科技有限公司 | Automated production line with modified fiber electromagnetic function |
| CN108702817B (en) * | 2016-02-15 | 2021-09-10 | 松下电器产业株式会社 | Method and apparatus for transmitting radio frequency electromagnetic energy for cooking foodstuff |
| CN106399977B (en) * | 2016-02-22 | 2022-03-25 | 河北陆元新材料科技有限公司 | Production system of coating silicon carbide composite fiber |
| CN109853089B (en) * | 2019-03-11 | 2021-10-12 | 施默尔(青岛)纤维复合材料有限公司 | High-performance carbon fiber and graphitization method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3607063A (en) * | 1969-10-09 | 1971-09-21 | United Aircraft Corp | Manufacture of carbon filaments of high strength and modulus |
| JPS54112214A (en) * | 1978-02-16 | 1979-09-03 | Toho Rayon Co Ltd | Production and device for high-tensile and high-modulus graphite fibers |
| JPS55163218A (en) * | 1979-11-12 | 1980-12-19 | Mitsubishi Rayon Co Ltd | Preparation of carbonaceous fiber |
| CN1060236C (en) * | 1998-06-15 | 2001-01-03 | 陈新谋 | Graphitized fiber manufacturing new process and special equipment |
| CN1442520A (en) * | 2002-03-05 | 2003-09-17 | 陈新谋 | One cavity multiple pipe high frequency heating device |
| CN1142333C (en) * | 2001-01-12 | 2004-03-17 | 陈新谋 | Carbin fibre graphitization process and its equipment |
-
2004
- 2004-04-19 CN CNB2004100122397A patent/CN1332082C/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3607063A (en) * | 1969-10-09 | 1971-09-21 | United Aircraft Corp | Manufacture of carbon filaments of high strength and modulus |
| GB1302058A (en) * | 1969-10-09 | 1973-01-04 | ||
| JPS54112214A (en) * | 1978-02-16 | 1979-09-03 | Toho Rayon Co Ltd | Production and device for high-tensile and high-modulus graphite fibers |
| JPS55163218A (en) * | 1979-11-12 | 1980-12-19 | Mitsubishi Rayon Co Ltd | Preparation of carbonaceous fiber |
| CN1060236C (en) * | 1998-06-15 | 2001-01-03 | 陈新谋 | Graphitized fiber manufacturing new process and special equipment |
| CN1142333C (en) * | 2001-01-12 | 2004-03-17 | 陈新谋 | Carbin fibre graphitization process and its equipment |
| CN1442520A (en) * | 2002-03-05 | 2003-09-17 | 陈新谋 | One cavity multiple pipe high frequency heating device |
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| CN1690261A (en) | 2005-11-02 |
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