CN106367849B - Serialization silicon carbide fibre production system - Google Patents

Serialization silicon carbide fibre production system Download PDF

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Publication number
CN106367849B
CN106367849B CN201610095628.3A CN201610095628A CN106367849B CN 106367849 B CN106367849 B CN 106367849B CN 201610095628 A CN201610095628 A CN 201610095628A CN 106367849 B CN106367849 B CN 106367849B
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gas
quartz tube
tube reactor
reaction
silk
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CN106367849A (en
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王敬霞
陈刚
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Hebei Lu Yuanxin Mstar Technology Ltd
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Hebei Lu Yuanxin Mstar Technology Ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/10Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The production system of continuous carbofrax fibre, purpose is that silicon carbide fibre principle device is prepared to high-frequency method improves design, to adapt to the needs of mass production, to guarantee that main technic index, such as precise coordination of reaction temperature, reacting gas concentration and carrier silk control, to solve the pollution that the stringent discreteness of finished silicon carbide product silk technical indicator required, controlled production cost and environment.The technical solution adopted is that: system composition in include be configured with the line focus device of radio-frequency power supply, the quartz tube reactor that linear focusing device axis line position is set, retractable silk mechanism, the guarantee of reaction environment atmosphere and processing unit and with the on-line monitoring of the above setted structure and management circuit.By the design of the guarantee of reaction environment atmosphere and processing unit, the accuracy controlling and meet the requirement of environmental protection of reacting gas concentration are realized, saves economic cost.

Description

Serialization silicon carbide fibre production system
Technical field
The invention belongs to produce the further perfect of silicon carbide fibre system based on vapour deposition process and radio frequency focusing device And supplement, experimental system is risen into the serialization silicon carbide fibre with complete production equipment and technology by practice of trial production Production system.
Background technique
Silicon carbide fibre is the ceramic material of a kind of high specific strength, high specific stiffness, high elastic modulus.Especially with tungsten wire For core material, the silicon carbide fibre obtained by means of vapour deposition process structure uniformly, stable physical-chemical indexes and have absorption electromagnetism The characteristic of wave and hot environment long-term work, thus it is widely applied to Aeronautics and Astronautics and a variety of military fields, it is each by the world The great attention of state.The states such as the U.S., West Germany begin to develop silicon carbide fibre from the seventies, produce the master of silicon carbide fibre Wanting technological principle is using vapour deposition process.So-called vapour deposition process uses tungsten wire as carrier, and carrier is being full of chlorine silicon 1100 ~ 1400 DEG C are warmed in the reactor of alkane one kind gas, gas is made to decompose and be formed with the structure of silicon carbide deposition, growth Tungsten core silicon carbide fibre.Since the diameter of carrier silk only has 10 μm or so, the silicon carbide fibre diameter that deposition becomes finished product is it Even hundreds times of several times decades of times, so the fiber formed is it may be said that substantially silicon carbide fibre.As it can be seen that in entire technique mistake Fundamental problem is to solve to be uniformly heated to 1100 ~ 1400 DEG C to carrier silk, and during continuous folding and unfolding silk, keep in journey The stability of this process conditions.Many methods can be had by being heated to 1200 DEG C or so to silk material.But join in chlorosilane gas Under conditions of adding reaction, we only need carrier itself to have this reaction temperature, if in the reaction chamber simultaneously there is also Other heat carriers directly reduce the conversion ratio of available gas, in other words then just having its surface of a large amount of depositing SiC It exactly wastes too big.So directly heating to carrier itself is unique soluble method.
Currently, one is grasped by the U.S., Japan and other countries to there are two types of the direct-fired common methods of silk material itself DC heating method, i.e., the directly logical upper direct current on carrier makes its own fever to reaction temperature, and corresponding equipment is Direct current method thermal reaction apparatus.This reaction unit is because will be arranged mercury seal electrode at quartzy thermal reactor both ends to guarantee to carry Body silk is well contacted with electrode, although ensure that silk material resistance value is constant in reaction zone, so that heating carrier silk temperature is constant, But mercury seal electrode can be because work generates mercury vapour and leakage is caused to endanger public security in the high temperature environment Solve the problems, such as that this needs to carry out whole device multiple-sealed, thus cost is high, and application is limited to.More seriously In the micro infiltration silicon carbide crystalline texture of mercury molecule, defect will form, cause to be converted into failure under high-strength stress Point.In addition, since deposition velocity is very fast, fiber outlet has larger with inlet fabric resistor value when preparing large-diameter fiber Difference, to keep the diameter mean square deviation of finished fiber higher, influences silk material so that the entry and exit temperature difference be made to reach 200 ~ 300 DEG C The physical application in high-precision product.
Another is that exactly inventor herein designs to the direct-fired method of silk material, and this method is using high frequency Actinobolia completes the heating to carrier instead of DC resistance method.Specific method is exactly to be formed on the axis of quartzy thermal response pipe One high frequency focused electromagnetic generated by radio frequency heating dedicated unit makes the tungsten wire in movement obtain untouchable heating, The reaction environment being made of the gaseous mixture of chlorosilane and high-purity hydrogen is produced in quartz tube reactor simultaneously, makes chlorine silicon Alkane generates depositing SiC in cracking in carbon fiber surface, forms coat of silicon carbide.And the hydrogen chloride generated in reacting is then arranged Reactor is absorbed by limewash out.In this way as carbon fiber continues through focused electromagnetic and is heated to 1100 DEG C ~ 1300 DEG C, The chlorosilane and high-purity hydrogen being filled with will react therewith forms one layer of coat of silicon carbide on the surface of carbon fiber.It is appropriate to grasp Silk and is filled with amount of reactant gases at speed, reaction temperature, can control the thickness of surface covering.
However, the model of the radio frequency heating reaction unit from the principle in the laboratory research stage, being converted into can be with It realizes the production system and process of complete process route, and is involved in more practical operating technology problem.Except want essence It really grasps and regulates and controls power match, wire travelling speed, reaction temperature and be filled with outside amount of reactant gases, to the stabilization of wire travelling speed, penetrate The problems such as stabilization of frequency heating system, the stabilization of reaction environment, exhaust-gas treatment, made higher requirement, this will affect entirely The continuous uninterrupted production of the production cost, production system of production system, avoid because frequently occur reaction environment, condition and Wire travelling speed is unstable to cause the non-uniform technical problem of finished product yarn quality.
How radio frequency heating method prepared into silicon carbide continuous fiber, complete process system is improved to by principle model, from And make the product of silicon carbide fibre formation mass production, it has also become the extremely urgent task of this project.
Summary of the invention
Present invention aims at preparing silicon carbide fibre principle device to high-frequency method to improve design, to adapt to mass The needs of production, to guarantee the precise coordination control of main technic index, such as reaction temperature, reacting gas concentration and carrier silk System, to solve the pollution that the stringent discreteness of finished silicon carbide product silk technical indicator required, controlled production cost and environment.This hair Bright design key is for the mating auto-control servo mechanism of serialization silicon carbide fibre high frequency focusing heating mechanism and guarantee System and technique make every effort to the accurate control for realizing volume production and fiber process, and realize connect with what world's environmental protection and energy saving required simultaneously Rail.
The present invention be realize goal of the invention the technical solution adopted is that:
The production system of continuous carbofrax fibre, system composition in include be configured with radio-frequency power supply line focus device, Quartz tube reactor, retractable silk mechanism, the guarantee of reaction environment atmosphere and the processing of linear focusing device axis line position are set Device and with the on-line monitoring of the above setted structure and management circuit, wrap in the guarantee of reaction environment atmosphere and processing unit structure It includes:
1. it is connected to the gas distribution assembly on the reaction gas air inlet of quartz tube reactor,
2. the recovery processing assembly being connected on the gas outlet of quartz tube reactor.
It include: the distribution at least two reaction gas air inlets and a gas outlet in the composition of the gas distribution assembly Cabinet, above-mentioned air inlet, gas outlet are connect by pipeline with the air inlet of respective reaction gas source or quartz tube reactor respectively, It is arranged in series controllable regulator valve and mass flowmenter in the pipeline, pressure sensor is set on distributing cabinet.
Reach the stringent discreteness requirement of silicon carbide fibre quality, the control of reaction environment atmosphere is the key that production. Make the silicon carbide production system of carrier for tungsten wire, the diameter difference of tungsten wire and finished silk probably at several times even tens times, because This, the finished fiber that tungsten wire does carrier can almost ignore tungsten wire and be considered silicon carbide fibre.It will be in quartz tube reactor It realizes and deposits a thick layer of silicon carbide, and guarantee the uniformity of depositing SiC from the inside to the outside and from the beginning to the end, need to consider Factors in, the regulation of reaction environment atmosphere is the key that the high-quality finished silk of production.
The guarantee of reaction environment atmosphere and processing unit include the regulation of reaction environment atmosphere, the regulation packet of reaction environment atmosphere The regulation for including gas concentration in quartz tube reactor, at the air inlet at the both ends of quartz ampoule thermal reactor and the gas outlet at middle part Place's configuration can adjust the controllable regulator valve of dynamic stability air pressure and gas mass flow meter in reactor.To obtain more Gao Pin The finished silk of matter considers to be become by minor diameter tungsten wire the variation of caused circumferential surface product when major diameter silicon carbide fibre, reaction Gas concentration at the air inlet at device both ends has the concentration difference of strict control.
The recycling of tail gas is purified and is recycled, and is the environmental requirement in order to reach world standard, while also can high degree Upper reduction economic cost.In quartz ampoule thermal reactor, cracking reaction and incomplete reaction occur for trichloromethyl silane and hydrogen Gas be possible to account for 40 or more percent, if cannot by tail gas recycle, generate hydrogen chloride gas leakage will Jeopardize the life of the entire production line worker, while unreacted trichloromethyl silane can also waste, causes greatly to pass through for enterprise Ji loss.The recovery processing circuit design of tail gas simultaneously also to a certain extent plays the easy-regulating of gas pressure in reactor Positive effect is arrived.
In addition the regulation of reaction environment atmosphere further includes the regulation of carrier silk thread speed and reaction temperature, and the two is plus quartz The regulation of gas concentration forms reaction environment atmosphere comprehensive regulation, the coordinated control between three, so that finished product in pipe reactor Silk has excellent discreteness.
The beneficial effects of the present invention are: (1) passes through the design of the guarantee of reaction environment atmosphere and processing unit, reaction is realized The accuracy controlling and meet the requirement of environmental protection of gas concentration save economic cost;(2) sealing device is blocked up by setting second level gas, It ensure that the safety and cleaning of reaction environment, while realizing the recycling or recycling and reusing of this expensive gases of argon gas;(3) lead to It crosses and is receiving silk end setting stepper motor and impulse controller, realize the speed stabilizing regulation of carrier silk;(4) by radio-frequency power supply Mating automated power adjusts device in structure, and adjustable sliding rail support, and setting are arranged on left and right conjugation resonant cavity Laser thermodetector realizes the accuracy controlling of reaction temperature.
The present invention is described in detail with reference to the accompanying drawing.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention (combination that Fig. 1 is Fig. 1 a and Fig. 1 b).
Fig. 2 is four-way second level plugging device and folding and unfolding silk mechanism and the connection schematic diagram of quartz tube reactor in the present invention.
In attached drawing, 1 represents radio-frequency power supply, and 1-1 represents automated power adjustment device, and 1-2,1-3 represent left and right conjugation resonance Chamber, 1-4,1-5 represent adjustable sliding rail support, and 2 represent quartz tube reactor, and 2-1 represents reaction gas air inlet, and 2-2 is represented Gas outlet, 2-3-1 represent reaction air cavity, and 2-3-2 represents sealed air-space, and 2-4 represents four-way second level plugging device, and 2-5 representative can Control regulation valve, 2-6 representation quality flowmeter, 3 represent distributing cabinet, 3-1 representative pressure sensor, and 4-1 represents cooling shunt and fills It sets, 4-2 represents water absorption tank, and 4-3 represents heating diversion cans, and 4-4 represents intermediate storage cabinet, and 5-1,5-2 represent retractable silk Wheel disc, 5-3 represent stepper motor, and 5-4 represents controlled pulse signal generator, and 6 represent laser thermodetector, in attached drawing, 1. represent The argon gas whereabouts of recycling.
Specific embodiment
Referring to Fig. 1, the production system of continuous carbofrax fibre includes being configured with the linear of radio-frequency power supply 1 in system composition Focusing device, the quartz tube reactor 2 that linear focusing device axis line position is set, retractable silk mechanism, reaction environment atmosphere Ensure and processing unit and with the on-line monitoring of the above setted structure and management circuit, the guarantee of reaction environment atmosphere and processing fill It sets in structure and includes:
1. it is connected to the gas distribution assembly on the reaction gas air inlet 2-1 of quartz tube reactor 2,
2. the recovery processing assembly being connected on the gas outlet 2-2 of quartz tube reactor 2.
It include: the distribution at least two reaction gas air inlets and a gas outlet in the composition of the gas distribution assembly Cabinet 3, above-mentioned air inlet, gas outlet are respectively by pipeline and respective reaction gas source or the air inlet 2-1 of quartz tube reactor 2 It connects, controllable regulator valve 2-5 and mass flowmenter 2-6 is arranged in series in the pipeline, pressure sensor 3- is set on distributing cabinet 3 1。
It is additionally provided with gas recovery inlet on the distributing cabinet 3, is connected on the gas outlet 2-2 of quartz tube reactor 2 Include: cooling part flow arrangement 4-1 in the equipment of recovery processing assembly, be connected on the diffluence pass of cooling part flow arrangement 4-1 Water absorption tank 4-2 and heating diversion cans 4-3, the hydrogen and trichloromethyl silane of recycling are respectively through intermediate storage cabinet 4-4's The gas recovery inlet of distributing cabinet 3 is communicated to after absorption impurity elimination, heating pressurization.
Reach the stringent discreteness requirement of silicon carbide fibre quality, the control of reaction environment atmosphere is the key that production. Make the silicon carbide production system of carrier for tungsten wire, the diameter difference of tungsten wire and finished silk probably at several times even tens times, because This, the finished fiber that tungsten wire does carrier can almost ignore tungsten wire and be considered silicon carbide fibre.It will be in quartz tube reactor It realizes and deposits a thick layer of silicon carbide, and guarantee the uniformity of depositing SiC from the inside to the outside and from the beginning to the end, need to consider Factors in, the regulation of reaction environment atmosphere is the key that the high-quality finished silk of production.
The guarantee of reaction environment atmosphere and processing unit include the regulation of reaction environment atmosphere, the regulation packet of reaction environment atmosphere The regulation for including gas concentration in quartz tube reactor, at the air inlet at the both ends of quartz ampoule thermal reactor and the gas outlet at middle part Place's configuration can adjust the controllable regulator valve of dynamic stability air pressure and gas mass flow meter in reactor.To obtain more Gao Pin The finished silk of matter considers to be become by minor diameter tungsten wire the variation of caused circumferential surface product when major diameter silicon carbide fibre, reaction Gas concentration at the air inlet at device both ends has the concentration difference of strict control, this be follow fibre circumference surface area variation and The special designing made.
The recycling of tail gas is purified and is recycled, and is the environmental requirement in order to reach world standard, while also can high degree Upper reduction economic cost.In quartz ampoule thermal reactor, cracking reaction and incomplete reaction occur for trichloromethyl silane and hydrogen Gas be possible to account for 40 or more percent, if cannot by tail gas recycle, generate hydrogen chloride gas leakage will Jeopardize the life of the entire production line worker, while unreacted trichloromethyl silane can also waste, causes greatly to pass through for enterprise Ji loss.The recovery processing circuit design of tail gas simultaneously also to a certain extent plays the easy-regulating of gas pressure in reactor Positive effect is arrived.
In addition the regulation of reaction environment atmosphere further includes the regulation of carrier silk thread speed and reaction temperature, and the two is plus quartz The regulation of gas concentration forms reaction environment atmosphere comprehensive regulation, the coordinated control between three, so that finished product in pipe reactor Silk has excellent discreteness.
The reaction chamber both ends of quartz tube reactor 2 are equipped with double partial pressure fluid resistant seal structures: respectively including by two mutually The reaction chamber of the duplex air cavity that three breather chambers of connection are formed, a gas outlet of the duplex air cavity and quartz tube reactor 2 into Port connection, another gas outlet is connected to quartz tube reactor 2 into and out of wire hole, and in duplex air cavity with reaction chamber air inlet Directly be connected to be connect gas distribution assembly reaction air cavity 2-3-1, with into and out of wire hole be connected to directly be connected to be connect seal argon The sealed air-space 2-3-2 of gas source, argon gas introduce sealed air-space by air inlet, by internal positive pressure dynamic is discharged, formed into and out of wire hole Turbulent flow type blanket gas is stifled.
Quartz tube reactor 2 into and out of being respectively provided with four-way second level envelope between wire hole end and retractable Si Liang mechanism Block apparatus 2-4, the both ends of quartz tube reactor 2 by attrition process at frosted conical head and above-mentioned four-way second level plugging device 2-4 realizes sealing docking, and high-purity hydrogen introduces from air inlet, draws from recovery port, forms the sealing of internal positive pressure dynamic turbulent flow type Structure.
The present invention one of them it is crucial that in quartz tube reactor into and out of being respectively equipped with double partial pressures inside and outside silk mouth port Fluid resistant seal structure and four-way second level plugging device.Double partial pressure fluid resistant seal structures use two three interconnected breather chambers, The mixed gas of the trichloromethyl silane and hydrogen of participating in reaction is passed through in the one or three breather chamber connecting with reactor, with disengaging It is passed through protection argon gas in two or three breather chamber of silk mouth end connection, while guaranteeing gas at the interconnected port of two three breather chambers Pressure, the one or three breather chamber react air cavity and are slightly larger than two or three breather chambers, that is, sealed air-space.Since argon gas is expensive, if can subtract Few argon gas by revealing into and out of silk outlet end, can also save production cost, therefore, in the disengaging silk of reactor to a certain extent It is additionally arranged a four-way second level plugging device respectively between mouth end and folding and unfolding silk mechanism, referring to Fig. 2, by being blocked by four-way second level The air inlet of device is passed through hydrogen, and air pressure at the port being connected to sealed air-space is made to be slightly less than sealed air-space, and argon gas is carried out Secondary plugging reduces the leakage of argon gas, has achieved the purpose that secondary seal, by the mixing of the hydrogen and argon gas of exhaust outlet discharge Gas can return to original production system by purification for argon machine.
The both ends of quartz tube reactor 2 are arranged in retractable silk mechanism, include retractable silk wheel disc 5-1,5-2 and resistance in structure Buddhist nun is tensioned wheel group structure.
Further include matched speed stabilizing guiding power-driven mechanism in the wire drawing mechanism, includes stepper motor 5-3 in structure With the controlled pulse signal generator 5-4 with management circuit connection.
The carrier silk used in the present invention is superfine tungsten wire, if drafting force it is unstable easily cause tungsten wire occur fracture and Product quality is uneven, it has to be forced to stop this production line.Therefore stepper motor and controlled is provided in wire drawing mechanism The linear velocity of pulse signal generator, strict control tungsten wire is stablized, also provided with D.C. regulated power supply, DC voltage stability degree It is can be controlled in 12v ± 0.01v, the speed of service of folding and unfolding silk mechanism can be made to stablize.
It is configured with automated power adjustment device 1-1 in the structure of radio-frequency power supply 1, includes pair in the structure of line focus device Claim left and right conjugation resonant cavity 1-2, the 1-3 being arranged on adjustable sliding rail support 1-4,1-5, left and right conjugation resonant cavity 1-2,1- Water cooling nested structure is set in 3.
It further include the laser thermodetector 6 for scanning 2 internal temperature of quartz tube reactor in the system, laser thermodetector 6 Signal feedback end and on-line monitoring and management circuit connection.
Automatic power-controlling device has been augmented in the structure of radio-frequency signal generator in radio-frequency power supply, can have been improved due to outer electric wave Dynamic and the loop of rf system component parameter minor change and the variation for leading to temperature in quartzy thermal reactor, to can guarantee fibre Tie up the stabilization of performance.This device takes out a signal from directional coupler, exports a signal by automatic power control system and uses To control the pumping signal for pushing circuit, to control the output signal of power amplifier, power amplifier can be made to keep a stabilization Power output.
To obtain efficient circuit matching and effectively eliminating end fuel factor, it is mounted at coupler both ends with permalloy material The Dual-barrel-shaped of material preparation couples screening arrangement.The inside and outside equal 120mm of pipe range, inner tube are directly sleeved on quartzy thermal reactor, inner tube with It couples cavity inner conductor to be isolated with polytetrafluoro ring, outer effective brass screw is directly anchored on the outer conductor of coupler to effectively eliminate Hold thermal response.
, can be using tungsten wire as carrier by device made of the above design concept, carrier silk is through retractable silk institutional adjustment Good axle center is overlapped.Start radio-frequency signal generator, and power output is adjusted according to operating temperature, reaction gas and protection can be passed through Gas, carrier silk are warming up to 1200 DEG C ~ 1400 DEG C immediately under high-frequency electromagnetic field action in reaction zone, with folding and unfolding silk mechanism Continuously run, silicon carbide uniform deposition on carrier i.e. generate synthesis silicon carbide fibre product.
Specifically, the valve and flowmeter that are first passed through on control piper before reaction are filled with reaction gas in the reactor, drive It drives the foreign gas in reactor out of, the gaseous mass analyzer detection in the preceding pipeline of cooling part flow arrangement 4-1 is set When foreign gas being not present into pipeline, high-purity argon gas is passed through by Ar inlet, guarantees the interconnected end of two three breather chambers Air pressure at mouthful, reaction air cavity are slightly larger than sealed air-space, avoid outside leakage of reaction gas to reactor, and make in two gas chambers Air pressure reaches dynamic equilibrium.Start radio frequency heating apparatus, and detects along reactor axis through laser scanner to each section temperature When degree all reaches standard requirements, with continuously running for folding and unfolding silk mechanism, silicon carbide uniform deposition generates synthesis on carrier Silicon carbide fibre product.
Exhaust outlet is equipped in the middle part of reactor, have in the gas being persistently discharged by exhaust outlet it is most of be trichloromethyl silane and Hydrogen, remaining is by-product and hydrogen chloride etc., cooling part flow arrangement 4-1 is arranged in recovery pipe, by the mixed of exhaust outlet discharge Gas is closed after cooling part flow arrangement 4-1, trichloromethyl silane and by-product are cooled to liquid and are delivered to heating diversion cans 4- 3, and hydrogen and hydrogen chloride are by the way that after water absorption tank 4-2, hydrogen chloride is then stored to centre by water or limewash absorption, hydrogen Cabinet 4-4, or be reused or make other purposes, in the present invention, it is sharp again that hydrogen can return to original system according to process requirement With entering original production system by the gas recovery inlet on distributing cabinet.The gaseous material come out by heating diversion cans 4-3 For trichloromethyl silane, and it is stored to intermediate storage cabinet, or is reused and returns to original system or make other purposes, in the present invention In, trichloromethyl silane can return to original system according to process requirement and recycle, that is, pass through the gas recovery inlet on distributing cabinet Into original production system.
Distributing cabinet 3 and controllable regulator valve and gas mass flow meter are added between quartz tube reactor and reactant gas source, It can guarantee that hydrogen and trichloromethyl silane inject quartz tube reactor with reasonable ratio, while can be according to gas mass flow The feedback of meter and the feedback of gas analyzer, real-time online adjust the opening degree of controllable regulator valve, so as to accurately controlling and Adjust air pressure and gas concentration in reactor.
In conclusion the beneficial effects of the present invention are: (1) by the design of the guarantee of reaction environment atmosphere and processing unit, The accuracy controlling and meet the requirement of environmental protection of reacting gas concentration are realized, economic cost is saved;(2) stifled by setting second level gas Sealing device, ensure that the safety and cleaning of reaction environment, while the recycling or recycling that realize this expensive gases of argon gas are again It utilizes;(3) by receiving silk end setting stepper motor and impulse controller, the speed stabilizing regulation of carrier silk is realized;(4) by Mating automated power adjusts device in the structure of radio-frequency power supply, and adjustable sliding rail branch is arranged on left and right conjugation resonant cavity Seat, and setting laser thermodetector, realize the accuracy controlling of reaction temperature.

Claims (5)

1. the production system of continuous carbofrax fibre, include in system composition the line focus device for being configured with radio-frequency power supply (1), Be arranged in the quartz tube reactor (2) of linear focusing device axis line position, retractable silk mechanism, the guarantee of reaction environment atmosphere and Processing unit and with the on-line monitoring of the above setted structure and management circuit, it is characterised in that: the guarantee of reaction environment atmosphere and Include: in processing unit structure
The gas distribution assembly being connected on the reaction gas air inlet (2-1) of quartz tube reactor (2),
The recovery processing assembly being connected on the gas outlet (2-2) of quartz tube reactor (2);
The reaction chamber both ends of quartz tube reactor (2) are equipped with double partial pressure fluid resistant seal structures: respectively including mutually being interconnected by two The duplex air cavity that logical three breather chambers are formed, the reaction chambers of a gas outlet of the duplex air cavity and quartz tube reactor (2) into Port connection, another gas outlet is connected to quartz tube reactor (2) into and out of wire hole, and in duplex air cavity with reaction chamber air inlet Mouth be directly connected to be connect gas distribution assembly reaction air cavity (2-3-1), be directly connected into and out of wire hole be connect seal argon The sealed air-space (2-3-2) of gas source, argon gas introduce sealed air-space by air inlet, are moved by being discharged into and out of wire hole, forming internal positive pressure State turbulent flow type blanket gas is stifled;
It include: the distributing cabinet at least two reaction gas air inlets and a gas outlet in the composition of the gas distribution assembly (3), above-mentioned air inlet, gas outlet are respectively by pipeline and respective reaction gas source or the air inlet of quartz tube reactor (2) (2-1) is connected, and is arranged in series controllable regulator valve (2-5) and mass flowmenter (2-6) in the pipeline, distributing cabinet is arranged on (3) Pressure sensor (3-1);
It is additionally provided with gas recovery inlet on the distributing cabinet (3), is connected on the gas outlet (2-2) of quartz tube reactor (2) Recovery processing assembly equipment in include: cooling part flow arrangement (4-1), be connected to cooling part flow arrangement (4-1) point Water absorption tank (4-2) and heating diversion cans (4-3), the hydrogen and trichloromethyl silane of recycling on head piece are deposited through centre respectively Absorption impurity elimination, the heating of container (4-4) are communicated to the gas recovery inlet of distributing cabinet (3) after pressurizeing;
Quartz tube reactor (2) is blocked into and out of being respectively provided with four-way second level between wire hole end and retractable Si Liang mechanism Device (2-4), the both ends of quartz tube reactor (2) by attrition process at frosted conical head and above-mentioned four-way second level block and fill It sets (2-4) and realizes sealing docking, high-purity hydrogen introduces from air inlet, draws from recovery port, forms internal positive pressure dynamic turbulent flow type Sealing structure.
2. the production system of continuous carbofrax fibre according to claim 1, it is characterised in that: the setting of retractable silk mechanism It include retractable silk wheel disc (5-1,5-2) and damping tensioning wheel group structure at the both ends of quartz tube reactor (2), in structure.
3. the production system of continuous carbofrax fibre according to claim 2, it is characterised in that: in the wire drawing mechanism also Including matched speed stabilizing guiding power-driven mechanism, including stepper motor (5-3) and controlled with management circuit connection in structure Pulse signal generator (5-4).
4. the production system of continuous carbofrax fibre according to claim 1, it is characterised in that: the knot of radio-frequency power supply (1) It is configured with automated power adjustment device (1-1) in structure, includes being symmetricly set on adjustable sliding rail in the structure of line focus device Left and right conjugation resonant cavity (1-2,1-3) on support (1-4,1-5), left and right conjugation resonant cavity (1-2,1-3) is middle to be arranged water cooling Nested structure.
5. the production system of continuous carbofrax fibre according to claim 1, it is characterised in that: further include in the system Scan the laser thermodetector (6) of quartz tube reactor (2) internal temperature, the signal feedback end of laser thermodetector (6) and online prison Survey and manage circuit connection.
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CN108385087B (en) * 2018-02-12 2020-02-14 中南大学 Method for continuously and rapidly preparing BN coating on surface of SiC fiber
CN112481601A (en) * 2020-11-26 2021-03-12 中国科学院金属研究所 Device and method for preparing tungsten-boron radiation-proof fiber by CVD method
CN115538157B (en) * 2022-10-27 2024-02-23 湖南博翔新材料有限公司 Method for producing carbon nanotube modified silicon carbide fiber by continuous vapor deposition method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1461821A (en) * 2002-05-31 2003-12-17 陈新谋 Process and equipment for coating silicon carblde on carbon fiber surface
CN101121577A (en) * 2007-05-28 2008-02-13 魏永芬 Method and device for realizing double-component coat on SiC fibre surface
CN102094260A (en) * 2009-12-09 2011-06-15 中国科学院兰州化学物理研究所 Method for preparing metal-doped silicon carbide-based fibers

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1461821A (en) * 2002-05-31 2003-12-17 陈新谋 Process and equipment for coating silicon carblde on carbon fiber surface
CN101121577A (en) * 2007-05-28 2008-02-13 魏永芬 Method and device for realizing double-component coat on SiC fibre surface
CN102094260A (en) * 2009-12-09 2011-06-15 中国科学院兰州化学物理研究所 Method for preparing metal-doped silicon carbide-based fibers

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