CN101121577A - Method and device for realizing double-component coat on SiC fibre surface - Google Patents
Method and device for realizing double-component coat on SiC fibre surface Download PDFInfo
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- CN101121577A CN101121577A CNA2007100620057A CN200710062005A CN101121577A CN 101121577 A CN101121577 A CN 101121577A CN A2007100620057 A CNA2007100620057 A CN A2007100620057A CN 200710062005 A CN200710062005 A CN 200710062005A CN 101121577 A CN101121577 A CN 101121577A
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Abstract
The present invention relates to a method and a device to realize double-set separating coating on the surface of SiC cellulose, which belongs to the deep working region to SiC cellulose. The method relies on a radio and focalizing heating device to heat a tungsten filament in the movement, and then uses the gas-phase deposit method to produce SiC cellulose; the technical process is: (1) the quartz tube heat reaction device is changed into three sealing separating zones; (2) the tungsten filament heated by a radio electric field passes through the three gas-phase deposit zones in turn; (3) SiC is deposited in the Zone I and then forms SiC cellulose level on the surface of the tungsten filament; (4) an inner coating component deposit is designed inside of Zone II and then is on the surface of SiC cellulose level; (5) an outer coating component deposit is designed inside of Zone III and then is on the surface of inner coating of SiC cellulose level. The matched special device is an improvement to the quartz tube heat reaction device in the radio and focalizing heating device; in particular to a double-directional sealing argon seal is arranged in the quartz tube reaction device; a discharge mouth for the gas after being reacted is arranged on the front part of the seal; and an intake mouth for the mixing gases to be reacted and a discharge mouth for the gas after being reacted are arranged on the rear part of the seal.
Description
Technical field
The present invention relates to the SiC fiber is carried out the technology of deep processing.Realize the method and the device of double-component coat specifically at the SiC fiber surface
Background technology
The SiC fiber becomes the first-selection of high strength composite with its distinctive high specific strength and the snappiness amount of touching, and is used widely.Particularly, especially occupy special status in the war industry in the Aeronautics and Astronautics field.But the price of itself is too expensive, can only use as the skeleton of matrix material.In order to improve it and composite base material, titanium for example, bonding strength must scribble the excessive layer of iron at the SiC fiber surface.In order to improve its absorptive character, will be coated with carbon coating on its surface to frequency electromagnetic waves.If it is good compound both to have required SiC fiber and titanium alloy to have, the absorptive character of pair radar wave are arranged again, just can not be completed with single coating so, need double-component coat, promptly internal surface is coated with iron, and outside surface is coated with carbon.The needs different according to the user, inside and outside coating have different material requirements.At present institute have technique means only be by SiC fiber existing manufacturing technique and device reprocess, cost height, efficient be low.The method and the device that are implemented in SiC fiber surface double-component coat have become problem anxious to be solved.
Summary of the invention
The objective of the invention is to design a method and a device of realizing double-component coat at the SiC fiber surface, it heats the tungsten filament in the motion by means of the radio frequency focusing formula heating unit that the inventor invented, and utilized vapour deposition process to generate the technological process of SiC fiber, make the manufacturing that when the SiC fiber production completes, realizes double-component coat at the SiC fiber surface.
Silicon carbide has good high-temperature adaptability and ideal intensity and hardness, but common method is difficult to realize the making of SiC fiber.The radio frequency focusing formula heating unit (patent No. ZL91109267.6) that the inventor invented and matching used complete processing be to make the SiC fiber and form the ideal technique means of coat layer.But do not find method and the isolated plant of realizing the technology match with the object of the invention up to now, become the research topic that this area scientific and technical personnel are made earnest efforts now.
Realize the method for double-component coat when the invention provides a kind of SiC of making fiber at the SiC fiber surface, this method is by radio frequency focusing formula heating unit the tungsten filament in the motion to be heated, and utilized vapour deposition process to generate the technological process of SiC fiber, its key Design is:
(1) the silica tube thermal reactor structure in the radio frequency focusing formula heating unit is transformed, is made its reacting by heating district have three by the airtight argon gas that charges in stifled of the argon gas independent vapour deposition district of seal isolation respectively,
(2) by means of give, the traction of wire drawing mechanism and the tungsten filament that focuses on the rf electric field heating be successively by three vapour deposition districts,
(3) the I district forms the district for the SiC layer of fibers, by in quartz tube reactor I district, importing the gas mixture that chlorosilane adds high-purity hydrogen along the tungsten filament travel direction, form the reaction atmosphere that a chlorosilane adds high-purity hydrogen, realize that by the chlorosilane cracking and when generating hydrogenchloride SiC is deposited on the tungsten filament surface and forms the SiC layer of fibers
(4) the II district is the undercoat district, the tungsten core SiC fiber that is continued heating enters quartz tube reactor II district, contain the gaseous feed of undercoat component and the gas mixture of gas catalyst or reductive agent along the importing of conjugated fibre travel direction, be deposited on the fibrolaminar surface of SiC by cracking or reduction reaction generation design undercoat component
(5) the III district is the external coating (EC) district, the internally coated tungsten core SiC fiber that has that is continued heating enters quartz tube reactor III district, the contrary direction importing of moving along conjugated fibre contains the gaseous feed of external coating (EC) component and the gas mixture of gas catalyst or reductive agent, is deposited on SiC layer of fibers undercoat top layer by cracking or the designed external coating (EC) component of reduction reaction generation.
Above design philosophy is fully aware of, reaction environment when making full use of ratio-frequency heating and vapour deposition generation SiC fiber exactly, segmentation control reaction atmosphere then can made the fibrolaminar deposition of finishing complicated SiC fiber surface double-component coat simultaneously of SiC.Obviously, another key of problem is how to transform conventional device, makes it adapt to above method.
The present invention has designed a kind of radio frequency focusing formula heating unit at SiC fiber surface realization double-component coat simultaneously, and this device comprises radio-frequency generator, radio frequency adaptation, radio frequency cable, RF-coupled chamber, quartz tube reactor, fiber folding and unfolding silk mechanism.The quartz tube reactor that is arranged in symmetrically arranged RF-coupled chamber that tungsten filament passes is an elongated tubular product such, pore long-neck shape is closed up at two ends, advancing, filament mouth neck inboard is respectively equipped with the stifled and argon gas inflation inlet of argon gas sealing of one-way sealing, in advancing of quartz tube reactor, the stifled inboard of argon gas sealing of filament mouth end one-way sealing is provided with the mixed gas of participating in vapor deposition reaction and adds inlet, be provided with reaction back gas exhaust port at quartz tube reactor middle part, crucial improvement is that be provided with the sealing of the argon gas of two way seal in the stage casing, radio frequency heating zone of quartz tube reactor stifled and be communicated with argon gas and fill with sealing is stifled, venting port.Forward position, the stifled place of argon gas sealing in set two way seal is a reaction back air scavenge mouth.Be provided with the mixed gas of participating in the undercoat vapor deposition reaction at the stifled place of argon gas sealing of set two way seal by the position, back and add inlet, the mixed gas that this mixed gas adds inlet and the reaction at former rear port place add set up a reaction between the inlet after the air scavenge mouth, three reaction mixture gas bodies add inlet and are connected with the reaction mixture gas body filling line of generation SiC layer of fibers, undercoat, external coating (EC) respectively successively.
Stifled and is communicated with ar gas acting by the argon gas sealing of set two way seal in the quartz tube reactor stage casing with sealing is stifled, the ratio-frequency heating district can be isolated into two, the rear is a coated areas, the place ahead is that the SiC layer of fibers generates and distinguishes.Because the venting port of coated areas is located at interlude, the gas-phase reaction mixed gas that participates in inside and outside coating advances to venting port with essentially identical pressure from the front-end and back-end input of this section respectively simultaneously, so can be that the boundary forms two vapour deposition district of inside and outside floor at this section, have satisfied the basic demand of processing method with newly-increased venting port.
The present invention can be according to the composition and the thickness of the inside and outside coating of customer requirements, producing the disposable processing request of finishing undercoat, external coating (EC) of fibrolaminar while of SiC, can simplify production process widely, reduce production costs, save energy, and institute's product processed coat-thickness control is strict, aspect is in conjunction with stable strong, and technical feature is stable.
Below in conjunction with accompanying drawing and provide embodiment and further specify and the objective of the invention is how to realize.
Description of drawings
Fig. 1 is the structural representation of radio frequency focusing formula heating unit.
Fig. 2 is the structural representation of the designed two inside-plugging silica tube thermal reactor embodiment among the present invention.
Number designation representative in the accompanying drawing: producer is frequently bended forward in 1 representative, 2 represent radio frequency adaptation, 3 represent radio frequency cable, the RF-coupled chamber of 4 representatives, 5 represent the silica tube thermal reactor, 51,52 represent the advancing of thermal reactor of silica tube, filament mouth, 53,54, the gas inlet of vapor deposition reaction is participated in 55 representatives, and 6 represent folk prescription stifled to the argon gas sealing of sealing, 61,62 represent the inlet of argon gas, 7,9 representative reaction back gas bleeding points, 8 represent the argon gas sealing of twocouese sealing stifled, and 81, on behalf of the stifled argon gas of argon gas sealing of twocouese sealing, 82 fill, venting port, 9 representative reaction back gas bleeding points, 10,11 represent fiber folding and unfolding silk mechanism, and 12 represent tungsten filament.
Embodiment
Can clearly find out male the present invention method designed, realize double-component coat at the SiC fiber surface by accompanying drawing, be the tungsten filament 12 in the motion to be heated by radio frequency focusing formula heating unit, and utilized vapour deposition process to generate the technological process of SiC fiber, critical step is:
(1) the silica tube thermal reactor structure in the radio frequency focusing formula heating unit is transformed, is made its reacting by heating district have three by the airtight argon gas that is charged in stifled of the argon gas independently vapour deposition district of seal isolation respectively,
(2) by means of give, the traction of wire drawing mechanism (10,11) and the tungsten filament 12 that focuses on the rf electric field heating be successively by three vapour deposition districts,
(3) the I district forms the district for the SiC layer of fibers, by in quartz tube reactor I district, importing the gas mixture that chlorosilane adds high-purity hydrogen along the tungsten filament travel direction, form the reaction atmosphere that a chlorosilane adds high-purity hydrogen, realize that by the chlorosilane cracking and when generating hydrogenchloride SiC is deposited on tungsten filament 12 surfaces and forms the SiC layer of fibers
(4) the II district is the undercoat district, the tungsten core SiC fiber that is continued heating enters quartz tube reactor II district, the working direction importing of moving along conjugated fibre contains the gaseous feed of undercoat component and the gas mixture of gas catalyst or reductive agent, be deposited on the fibrolaminar surface of SiC by cracking or the designed interior coating ingredients of reduction reaction generation
(5) the III district is the external coating (EC) district, the internally coated tungsten core SiC fiber that has that is continued heating enters quartz tube reactor III district, contain the gaseous feed of external coating (EC) component and the gas mixture of gas catalyst or reductive agent along the contrary direction importing of conjugated fibre progressive, be deposited on SiC layer of fibers undercoat top layer by cracking or the designed external coating (EC) component of reduction reaction generation.
According to the data statistics that goes out of experiment repeatedly, radio frequency focusing formula heating unit is heated tungsten filament and is maintained realization vapor deposition reaction process under 900 ℃-1400 ℃.
Tungsten filament in the motion produces the linear velocity of 0.5-1.5 meter per second under the guiding of retractable silk mechanism.
The SiC layer of fibers form produce in the district the required atmosphere of SiC layer of fibers deposition be by flow be 200-500 ml/min dimethyldichlorosilane(DMCS), flow be the monomethyl trichlorosilane of 600-1500 ml/min and high-purity hydrogen that flow is the 900-2300 ml/min inject that mixing tank is mixed and pressure regulation after inject this district and form.
SiC layer of fibers undercoat forms and to produce the required atmosphere of undercoat deposition in the II district, district is that flow is the gaseous state iron trichloride of 100-200 ml/min with flow is the 50-100 ml/min high-purity hydrogen injects mixing tank and is mixed that this district of injection forms after the also pressure regulation.
SiC layer of fibers external coating (EC) forms and to produce the required atmosphere of external coating (EC) deposition in the district is that flow is that the acetylene of 100-200 ml/min injects and injects this district after the mixing tank pressure regulation and form.
More than the purity of said high-purity hydrogen reach 99.9999%.
From the airtight argon gas amount of charging into that charges into stifled of argon gas is the 500-1200 ml/min, charges into the environmental stress that air pressure is not less than each adjacent vapour deposition district in the silica tube.
Referring to accompanying drawing clearly silkworm go out with present method supporting, in the radio frequency focusing formula heating unit mechanism of SiC fiber surface realization double-component coat, comprise radio frequency generators 1, radio frequency adaptation 2, radio frequency cable 3, RF-coupled chamber 4, quartz tube reactor 5, fiber folding and unfolding silk mechanism (10,11) form, tungsten filament 12 passes the quartz tube reactor 5 that claims in the RF-coupled chamber 4 and is elongated tubular, pore long-neck shape is closed up at two ends, advancing, filament mouth (51,52) the neck inboard is respectively equipped with the argon gas sealing stifled 6 and the argon gas inflation inlet (61 of one-way sealing, 62), in advancing of quartz tube reactor 5, filament mouth (51,52) stifled 6 inboards of argon gas sealing of the one-way sealing that is provided with of end are provided with the mixed gas of participating in vapor deposition reaction and add inlet (53,55), be provided with reaction back gas bleeding point 7 at quartz tube reactor 5 middle parts, crucial improvement design is to be provided with in the stage casing, radio frequency heating zone of quartz tube reactor 5 the argon gas sealing stifled 8 of two way seal and is communicated with argon gas with sealing stifled 8 fills, venting port (81,82), in the forward position, stifled 8 places of argon gas sealing of set two way seal is reaction back air scavenge mouth 7, be provided with the mixed gas of participating in vapor deposition reaction at stifled 8 places of argon gas sealing of set two way seal by the position, back and add inlet 54, add inlet (54 at mixed gas, 55) set up reaction back air scavenge mouth 9 between, the reaction mixture gas body adds inlet (53,54,55) successively respectively with generate the SiC layer of fibers, undercoat, the reaction mixture gas body filling line that is coated with vapor deposition layer outward connects.
The argon gas that charges into argon gas sealing stifled (6,8) from the argon gas inlet is the positive pressure of air pressure a little more than the hybrid reaction gaseous tension, so can realize the hermetic seal to silica tube.Increase the two way seal that is provided with stifled 8 the heating zone of argon gas sealing with silica tube be divided into two districts, one is the fibrolaminar reactive deposition of SiC district, reacted gas clump adds venting port 7 and discharges, one then is undercoat and the gas-phase reaction sedimentary province that is coated with outward, charge into mouthful 54 owing to after the argon gas of two way seal sealing stifled 8, set up one as internally coated gas-phase reaction gas in the Hou Yi district, charge into the gas-phase reaction gas of external coating (EC) this moment from inflation inlet 55, and adjust the pressure unanimity of two kinds of mixed gass, just can guarantee that with newly-increased venting port be that the boundary is in this section forms, outer two vapour deposition districts have satisfied the basic demand of processing method.
Further improvement project is the argon gas sealing stifled (8) that two two way seals are set, each sealing is stifled all to be provided with and to be communicated with the filling of argon gas pipeline, venting port (81,82), the argon gas of the two way seal that is increased sealing stifled (8) is arranged on gas port (54 after the gas-phase reaction, 55) in the middle of, abut against after two reactions between the gas discharge outlet (9).
Claims (10)
1. realize the method for double-component coat at the SiC fiber surface, this method is by radio frequency focusing formula heating unit the tungsten filament (12) in the motion to be heated, and has utilized vapour deposition process to generate the technological process of SiC fiber, it is characterized in that:
(1) the silica tube thermal reactor structure in the radio frequency focusing formula heating unit is transformed, is made its reacting by heating district have three by the airtight argon gas that is charged in stifled of the argon gas independent vapour deposition district of seal isolation respectively,
(2) by means of give, the traction of wire drawing mechanism (10,11) and the tungsten filament (12) that focuses on the rf electric field heating be successively by three vapour deposition districts,
(3) the I district forms the district for the SiC layer of fibers, form the reaction atmosphere that a chlorosilane adds high-purity hydrogen by in quartz tube reactor I district, importing the gas mixture that chlorosilane adds high-purity hydrogen along the tungsten filament travel direction, realize that by the chlorosilane cracking and when generating hydrogenchloride SiC is deposited on tungsten filament (12) surface and forms the SiC layer of fibers
(4) the II district is the undercoat district, the tungsten core SiC fiber that is continued heating enters quartz tube reactor II district, the working direction importing of moving along conjugated fibre contains the gaseous feed of undercoat component and the gas mixture of gas catalyst or reductive agent, be deposited on the fibrolaminar surface of SiC by cracking or the designed interior coating ingredients of reduction reaction generation
(5) the III district is the external coating (EC) district, the internally coated tungsten core SiC fiber that has that is continued heating enters quartz tube reactor III district, and the gas mixture that imports the gaseous feed that contains the external coating (EC) component and gas catalyst or reductive agent along the contrary direction of conjugated fibre progressive is deposited on SiC layer of fibers undercoat top layer by cracking or the designed external coating (EC) component of reduction reaction generation.
2. according to the said method of claim 1, it is characterized in that radio frequency focusing formula heating unit is heated tungsten filament and realized vapor deposition processes down at 900 ℃-1400 ℃ at SiC fiber surface realization double-component coat.
3. realize the method for double-component coat according to claim 1 is said at the SiC fiber surface, the tungsten filament in it is characterized in that moving send, produce under the guiding of wire drawing mechanism 0.5-1.5 rice/minute linear velocity.
4. realize the method for double-component coat according to claim 1 is said at the SiC fiber surface, it is characterized in that the SiC layer of fibers form produce in the district the required atmosphere of SiC layer of fibers deposition be by flow be 200-500 ml/min dimethyldichlorosilane(DMCS), flow be the monomethyl trichlorosilane of 600-1500 ml/min and high-purity hydrogen that flow is the 900-2300 ml/min inject that mixing tank is mixed and pressure regulation after inject this district and form.
5. realize the method for double-component coat according to claim 1 is said at the SiC fiber surface, it is characterized in that SiC layer of fibers undercoat form produce in the district the required atmosphere of undercoat deposition be flow is the gaseous state iron trichloride of 100-200 ml/min with flow is the 50-100 ml/min high-purity hydrogen inject that mixing tank is mixed and pressure regulation after this district of injection form.
6. realize the method for double-component coat according to claim 1 is said at the SiC fiber surface, it is characterized in that SiC layer of fibers external coating (EC) forms that to produce the required atmosphere of external coating (EC) deposition in the district be that flow is that the acetylene of 100-200 ml/min injects and injects this district after the mixing tank pressure regulation and form.
7. according to claim 4 or 5 said methods, it is characterized in that the purity of said high-purity hydrogen reaches 99.9999% at SiC fiber surface realization double-component coat.
8. realize the method for double-component coat at the SiC fiber surface for one kind, it is characterized in that from the airtight argon gas amount of charging into that charges into stifled of argon gas be the 500-1200 ml/min, charge into the environmental stress that air pressure is not less than each adjacent vapour deposition district in the silica tube.
9. radio frequency focusing formula heating unit of realizing double-component coat at the SiC fiber surface, this device comprises radio frequency generators (1), radio frequency adaptation (2), radio frequency cable (3), RF-coupled chamber (4), quartz tube reactor (5), fiber send, wire drawing mechanism (10,11), it is elongated tubular that tungsten filament (12) passes the quartz tube reactor (5) that claims in the RF-coupled chamber (4), pore long-neck shape is closed up at these pipe two ends, advancing, filament mouth (51,52) the neck inboard is respectively equipped with argon gas sealing stifled (6) and the argon gas inflation inlet (61 of one-way sealing, 62), in advancing of quartz tube reactor (5), stifled (6) inboard of argon gas sealing of the one-way sealing that the filament mouth end is provided with is provided with the mixed gas of participating in vapor deposition reaction and adds inlet (53,55), be provided with reaction back gas bleeding point (7) at quartz tube reactor (5) middle part, it is characterized in that interlude in the radio frequency heating zone of quartz tube reactor (5) is provided with the argon gas sealing stifled (8) of two way seal and is communicated with argon gas with sealing stifled (8) fills, venting port (81,82), locating forward position in the argon gas sealing stifled (8) of set two way seal is reaction back air scavenge mouth (7), locate to be provided with the mixed gas of participating in vapor deposition reaction in the argon gas sealing stifled (8) of set two way seal and add inlet (54) by the position, back, add inlet (54 at mixed gas, 55) set up reaction back air scavenge mouth 9 between, the reaction mixture gas body adds inlet (53,54,55) successively respectively with generate the SiC layer of fibers, undercoat, the reaction mixture gas body filling line that is coated with vapor deposition layer outward connects.
10. according to the said radio frequency focusing formula of claim 9 heating unit, the argon gas sealing stifled (8) that it is characterized in that said two way seal is provided with two on silica tube, each sealing is stifled to be provided with and to be communicated with the filling of argon gas pipeline, venting port (81,82), the argon gas of the two way seal that is increased sealing stifled (8) is arranged in the middle of the gas-phase reaction gas inflated mouth (54,55), abut against after two reactions between the gas discharge outlet (9).
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| CN106367849A (en) * | 2016-02-22 | 2017-02-01 | 河北陆元新材料科技有限公司 | Continuous silicon carbide fiber production system |
| CN106399977A (en) * | 2016-02-22 | 2017-02-15 | 河北陆元新材料科技有限公司 | Production system for coating silicon carbide composite fibers |
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| CN1033449C (en) * | 1991-10-05 | 1996-12-04 | 石家庄市电子加工技术研究所 | High-frequency thermal reactor for silicon carbide fibre |
| CN1047147C (en) * | 1995-09-29 | 1999-12-08 | 中国科学院山西煤炭化学研究所 | Method for production of coated silicon carbide fibre and reactor thereof |
| CN2283068Y (en) * | 1996-11-25 | 1998-06-03 | 中国科学院金属研究所 | Chemical vapour deposition silicon carbide fibre reactor |
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| CN106367849A (en) * | 2016-02-22 | 2017-02-01 | 河北陆元新材料科技有限公司 | Continuous silicon carbide fiber production system |
| CN106399977A (en) * | 2016-02-22 | 2017-02-15 | 河北陆元新材料科技有限公司 | Production system for coating silicon carbide composite fibers |
| CN106367849B (en) * | 2016-02-22 | 2019-05-17 | 河北陆元新材料科技有限公司 | Serialization silicon carbide fibre production system |
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| CN111172519A (en) * | 2020-01-17 | 2020-05-19 | 中国航发北京航空材料研究院 | Device and method for continuously preparing composite interface layer on surface of silicon carbide fiber |
| CN115896737A (en) * | 2022-11-17 | 2023-04-04 | 航天特种材料及工艺技术研究所 | High-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber and preparation method thereof |
| CN115896737B (en) * | 2022-11-17 | 2024-09-24 | 航天特种材料及工艺技术研究所 | High-temperature-resistant wave-absorbing tungsten/carbon-core silicon carbide fiber and preparation method thereof |
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