CN111005206B - Inorganic fiber precursor crosslinking curing method and device - Google Patents
Inorganic fiber precursor crosslinking curing method and device Download PDFInfo
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- CN111005206B CN111005206B CN201911329467.XA CN201911329467A CN111005206B CN 111005206 B CN111005206 B CN 111005206B CN 201911329467 A CN201911329467 A CN 201911329467A CN 111005206 B CN111005206 B CN 111005206B
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- 239000012701 inorganic fiber precursor Substances 0.000 title claims abstract description 70
- 238000004132 cross linking Methods 0.000 title claims abstract description 29
- 238000001723 curing Methods 0.000 title claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 77
- 238000001816 cooling Methods 0.000 claims abstract description 36
- 238000010894 electron beam technology Methods 0.000 claims abstract description 34
- 239000000835 fiber Substances 0.000 claims abstract description 29
- 239000011261 inert gas Substances 0.000 claims abstract description 29
- 239000002826 coolant Substances 0.000 claims description 33
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 25
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 22
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 17
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 230000005540 biological transmission Effects 0.000 claims description 15
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 11
- 239000004917 carbon fiber Substances 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- 239000001307 helium Substances 0.000 claims description 9
- 229910052734 helium Inorganic materials 0.000 claims description 9
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000003507 refrigerant Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000012784 inorganic fiber Substances 0.000 claims description 7
- 239000003570 air Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 239000012267 brine Substances 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 3
- 238000012806 monitoring device Methods 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 abstract description 7
- 230000008018 melting Effects 0.000 abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 229920005594 polymer fiber Polymers 0.000 description 33
- 239000011229 interlayer Substances 0.000 description 12
- 238000007789 sealing Methods 0.000 description 6
- 230000017525 heat dissipation Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000005192 partition Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 229920006253 high performance fiber Polymers 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910000952 Be alloy Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/005—Laser beam treatment
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- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Fibers (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The application relates to an inorganic fiber precursor crosslinking curing method, which comprises the following steps: firstly, placing inorganic fiber precursors arranged in the same orientation in a vacuum state; and secondly, placing the inorganic fiber precursor under inert gas atmosphere for electron beam irradiation to obtain the crosslinked and solidified inorganic fiber precursor. The application also designs a net tray collecting device which enables the inorganic fiber precursors to be arranged according to the same orientation, the device is arranged in a closed box body which can realize vacuum state and inert gas atmosphere, thereby avoiding the influence of oxygen on the fiber precursors, being beneficial to the rapid dissipation of heat, and being provided with a cooling system for further rapidly dissipating heat, avoiding the melting of the fiber precursors.
Description
Technical Field
The application relates to the technical field of fiber material treatment, in particular to a crosslinking and curing method and device for inorganic fiber precursor.
Background
Inorganic high-performance fibers such as silicon carbide fibers, silicon nitride fibers, carbon fibers and the like are typical representatives of high temperature resistance, high mechanical strength and corrosion resistance at present, and have unique application values in the fields of engineering material modification, engines, aerospace, ships, nuclear power equipment and the like. The main processes for preparing the inorganic fiber comprise preparation of a precursor, precursor spinning, solidification of fiber precursor and sintering or carbonization of the fiber precursor. The difficulty is that the solidification of the fiber precursor, namely, how to carry out chemical crosslinking and chemical reconstruction under the condition of maintaining the appearance of the fiber precursor, so as to ensure that the inorganic high-performance fiber with stable and excellent properties is obtained in the sintering process.
Taking silicon carbide fiber precursor polymer as an example, three methods of oxygen, chemical vapor and electron irradiation are mainly used for curing the silicon carbide polymer fiber precursor. Of these, electron irradiation is the most direct curing method, however, absorption of energy by the polymer precursor during irradiation causes a temperature rise, which tends to cause melting of the fiber precursor and loss of the fiber structure. In addition, the fiber collection method commonly used at present is a roller method, namely, the fiber polymer precursor is collected on a roller, and the problems of uneven irradiation, heat concentration, slow heat dissipation, high cost and the like exist.
Disclosure of Invention
The application aims to solve the problems of uneven irradiation, concentrated heat, slow heat dissipation and high cost existing in the current electron irradiation process of inorganic fiber precursors, and provides a crosslinking and curing method and device of the inorganic fiber precursors.
In order to achieve the above object, the present application provides a method for crosslinking and curing inorganic fiber filaments, comprising the steps of: s1, arranging inorganic fiber precursors in the same orientation; s2, placing the inorganic fiber precursor in the step S1 in a vacuum state, and then placing the inorganic fiber precursor in an inert gas atmosphere; and S3, irradiating the inorganic fiber precursor after the step S2 by using an electron beam to obtain the crosslinked and solidified inorganic fiber precursor.
As a further improvement of the present application, in step S2, the degree of vacuum of the vacuum state<10 -3 Pa, the inorganic fiber precursor is placed in the vacuum state for a time of at least 2 hours.
As a further improvement of the present application, in the step S2, the vacuum degree of the inert gas atmosphere is maintained at 10Pa to 10 4 Pa.
As a further improvement of the present application, in step S2, the inert gas is any one of nitrogen, argon and helium.
As a further improvement of the application, in the step S3, the irradiation energy of the electron beam is 5 MGy-50 MGy, and the irradiation time is 5 min-80 min.
As a further improvement of the present application, the diameter of the inorganic fiber filaments is controlled to be 3 μm to 30 μm.
The application also provides a device for crosslinking and solidifying the inorganic fiber precursor, which comprises an electron beam irradiation system, a closed box body arranged under the electron beam irradiation system and provided with a transmission window, and a net tray collecting device arranged in the closed box body and used for arranging the inorganic fiber precursor in the same orientation, wherein a vacuumizing gas outlet connected with a vacuum system and an inert gas inlet filled with inert gas are arranged on the closed box body, and a cooling system used for cooling the inorganic fiber precursor is arranged close to the outer side of the closed box body.
As a further improvement of the application, the vacuum system comprises a vacuum pumping unit connected to the gas outlet and an inert gas injection unit connected to the inert gas inlet.
As a further improvement of the application, the cooling system is realized by arranging a sealing cooling interlayer connected with the cooling medium inlet and the cooling medium outlet on the outer side of the closed box body.
As a further improvement of the application, the medium introduced at the cooling medium inlet is any one of water, brine, alcohol-water mixture, oil, air, argon, helium and refrigerant.
The application has the beneficial effects that the application provides a crosslinking curing method of inorganic fiber precursor, wherein the inorganic fiber precursor arranged in the same orientation is firstly placed in a vacuum state and then is placed in an inert gas atmosphere for electron beam irradiation, so as to obtain the crosslinking curing inorganic fiber precursor. The application also designs an inorganic fiber precursor crosslinking curing device, which utilizes a net disk collecting device to ensure that fiber precursors are distributed in the same orientation, and compared with the traditional drum-type collecting device, the device can be more uniformly irradiated by electron beams; the introduction of the cooling system is beneficial to heat transmission and avoids the melting of the fiber precursor; the introduction of the vacuum system can avoid the influence of oxygen on the fiber precursor, and can effectively realize the rapid dissipation of heat, thereby further avoiding the melting of the fiber precursor. The method has spectrum adaptability, can realize the crosslinking and curing of the silicon carbide fiber precursor, the silicon nitride fiber precursor and the carbon fiber precursor, and can also be used for the crosslinking and curing of other inorganic fiber precursors, and the method is simple and has low cost.
Drawings
FIG. 1 is a block diagram of an inorganic fiber precursor crosslinking curing apparatus;
FIG. 2 is a block diagram of one embodiment of a cooling medium circulation flow path structure within a sealed cooling jacket;
FIG. 3 is a block diagram of another embodiment of a cooling medium circulation flow path structure within a sealed cooling jacket;
FIG. 4 is a block diagram of another embodiment of a cooling medium circulation flow path structure within a sealed cooling jacket;
in the figure: 1. an electron beam irradiation system; 2. a transmission window; 3. a closed box body; 4. inorganic fiber precursors; 5. a net tray collecting device; 6. a gas outlet; 7. an inert gas inlet; 8. sealing and cooling the interlayer; 9. a cooling medium inlet; 10. and a cooling medium outlet.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be clearly and completely described below with reference to specific embodiments of the present application and corresponding drawings. It will be apparent that the described embodiments are only some, but not all, embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
In order to solve the problems of uneven irradiation, concentrated heat, slow heat dissipation and high cost in the current electron irradiation process of the inorganic fiber precursor, the application provides an inorganic fiber precursor crosslinking and curing method, which comprises the following steps: s1, arranging inorganic fiber precursors in the same orientation, wherein the inorganic fiber precursors are preferably uniformly arranged in the same orientation, and the uniform arrangement mode of the orientation is beneficial to uniform irradiation of electron beams, and the inorganic fiber precursors are any one of silicon carbide polymer fiber precursors, silicon nitride polymer fiber precursors, carbon fiber precursors and the like; preferably, the diameter of the inorganic fiber precursor is controlled to be 3-30 μm; further, the inorganic fiber precursor is arranged in the same orientation by utilizing a net disk collecting device, and the collecting distance and the precursor concentration can be adjusted in the collecting process to obtain inorganic fiber precursor with different diameters; s2, firstly, placing the inorganic fiber precursor in the step S1 in a vacuum state for a period of time, and secondly, placing the inorganic fiber precursor in an inert gas atmosphere; further, the inorganic fibers are placed in a sealed box body, the sealed box body is vacuumized to achieve a vacuum state, and the vacuumization function is to verify the air tightness of the sealed box body and prevent air leakage on one hand and to eliminate the influence of oxygen on fiber precursors on the other hand; filling a proper amount of inert gas into the closed box body, wherein the inert gas is used for increasing the heat conduction between the inorganic fiber precursor collecting device and the box body so as to dissipate heat; and S3, irradiating the inorganic fiber precursor after the step S2 by using an electron beam to obtain the crosslinked and solidified inorganic fiber precursor. In addition, a further rapid heat dissipation step is additionally arranged in the irradiation process of the inorganic fiber precursor, and the rapid heat dissipation step is realized by arranging a cooling system on the outer side of a sealed box body for placing the inorganic fiber precursor.
In the application, further, the vacuum degree of the vacuum state<10 -3 Pa, the inorganic fiber filaments are maintained in the vacuum state for at least 2 hours; further, the vacuum degree of the inert gas atmosphere is maintained between 10Pa and 10Pa 4 Between Pa; in step S2, the inert gas is any one of nitrogen, argon, helium, and the like; in the step S3, the irradiation energy of the electron beam is 5 MGy-50 MGy; preferably, the irradiation energy of the electron beam is 8 MGy-18 MGy; the irradiation time is 5 min-80 min; preferably, the irradiation time is 20 min-50 min.
In the application, as shown in figure 1, a device for a crosslinking and solidifying method of inorganic fiber precursor comprises an electron beam irradiation system 1, a closed box body 3 arranged below the electron beam irradiation system 1 and provided with a transmission window 2, and a net tray collecting device 5 arranged in the closed box body 3 and enabling inorganic fiber precursor 4 to be arranged in the same orientation, wherein the size of the net tray collecting device 5 is matched with that of the closed box body 3, a vacuumizing gas outlet 6 connected with a vacuum system and an inert gas inlet 7 for injecting inert gas are arranged on the closed box body 3, a cooling system for cooling the inorganic fiber precursor 4 is arranged outside the closed box body 3 in a close fit manner, and a sealing cooling interlayer 8 connected with a cooling medium inlet 9 and a cooling medium outlet 10 is arranged outside the closed box body 3; further, the transmission window 2 is generally disposed at the top of the closed box body 3, so as to facilitate electron beam irradiation, the net disc collecting device 5 is generally disposed at the bottom of the closed box body 3, the sealing cooling interlayer 8 is closely attached to the outer side of the bottom of the closed box body 3, so that heat diffusion of the net disc collecting device 5 is facilitated, and further, the vertical distance between the net disc collecting device 5 and the transmission window 2 is less than 5cm.
In the application, the material of the transmission window is any one of titanium alloy, beryllium alloy and the like, so that electron beams can pass through conveniently; the vacuum system comprises a vacuumizing unit connected with the gas outlet 6 and an inert gas injection unit connected with the inert gas inlet 7, wherein the vacuumizing unit and the inert gas injection unit are independently controlled, and each subsystem is independently operated and freely assembled, so that the crosslinking and curing cost of the inorganic fiber precursor is further reduced; the application is also provided with a monitoring device for monitoring the vacuum degree of the closed box body 3 in real time; the cooling system is a circulating cooling system for circulating the medium; the medium is any one of water, brine, alcohol-water mixture, oil, air, argon, helium, refrigerant and the like, and the refrigerant is any one of Freon, R134A refrigerant, R22 refrigerant, R407C refrigerant, R410A refrigerant and the like.
In the present application, there are provided 3 examples of the form of circulation flow of the cooling medium in the seal-cooling interlayer 8: as shown in fig. 2, a pipeline circulation type cooling medium conveying channel is arranged in the sealing cooling interlayer 8, pipelines are uniformly distributed in the sealing cooling interlayer 8 in an S shape, one end of each pipeline is connected with a cooling medium inlet 9, the other end of each pipeline is connected with a cooling medium outlet 10, and the heat transfer of the inorganic fiber precursors is facilitated due to the arrangement of the S-shaped pipelines; as shown in fig. 3, the sealed cooling interlayer 8 is internally provided with baffle plate circulation type cooling medium conveying channels, the sealed cooling interlayer 8 is internally provided with baffle plates which are arranged at intervals to form an S-shaped channel which is convenient for the uniform circulation of the cooling medium, one end of the S-shaped channel is connected with the cooling medium inlet 9, and the other end is connected with the cooling medium outlet 10; as shown in fig. 4, the sealed cooling interlayer 8 is internally provided with a cooling medium conveying channel with converging partition boards, the sealed cooling interlayer 8 is internally provided with the partition boards which are arranged in a crossing way according to different directions, an S-shaped channel which is convenient for the converging circulation of the cooling medium is formed, one end of the channel is connected with the cooling medium inlet 9, the other end is connected with the cooling medium outlet 10, in the S-shaped channel, the interlayer space between the partition boards is narrow at one end and wide at the other end, the wide inlet and the narrow outlet of the cooling medium are formed, the residence time of the cooling medium in the channel is prolonged, and the heat transfer of the inorganic fiber precursors is facilitated.
In order to verify the technical effects of the present application, the following examples are provided, and the device provided by the present application is applied to crosslink and cure different fiber precursors, and the optimal process parameters are given, which are as follows:
example 1
The silicon carbide polymer fiber precursor is collected in a net tray collecting device, the arrangement of the silicon carbide polymer fiber precursor is parallel to two sides of the net tray, and the diameter of the obtained silicon carbide polymer fiber precursor is 3 mu m by adjusting the collecting distance and the precursor concentration between the net tray and the filament making equipment. Firstly, placing a net tray collecting device for collecting silicon carbide polymer fiber precursors into a closed box body provided with a transmission window; secondly, vacuumizing the closed box body to ensure that the initial vacuum degree of the container is 10 -4 Pa, continuing for 5 hours under the initial vacuum degree, then injecting helium gas to ensure that the pressure in the closed box body is 50Pa, starting a cooling system, adopting water as a medium, and ensuring that the flow speed is 50m 3 /h; and finally, starting an electron beam irradiation system to irradiate the silicon carbide polymer fiber precursor for 80 minutes under the irradiation energy of the electron beam of 5MGy, so as to obtain the crosslinked cured silicon carbide polymer fiber precursor with uniform and stable quality. This embodiment employs a pipe circulation type cooling medium conveying passage structure.
Example 2
The silicon carbide polymer fiber precursor is collected in a net tray collecting device, the arrangement of the silicon carbide polymer fiber precursor forms an included angle of 45 degrees with one side of the net tray, and the diameter of the obtained silicon carbide polymer fiber precursor is 30 mu m by adjusting the collecting distance between the net tray and the filament manufacturing equipment and the concentration of the precursor. Firstly, placing a net tray collecting device for collecting silicon carbide polymer fiber precursors into a closed box body provided with a transmission window; secondly, the closed box body is vacuumized to ensure that the initial vacuum degree of the container is 5 multiplied by 10 - 4 Pa, continuing for 3 hours under the initial vacuum degree, then injecting helium gas to enable the pressure in the closed box body to be 100Pa, starting a cooling system, adopting freon as a medium, and enabling the flow speed to be 25m 3 /h; and finally, starting an electron beam irradiation system to irradiate the silicon carbide polymer fiber precursor for 5 minutes under the irradiation energy of 50MGy electron beams, so as to obtain the crosslinked cured silicon carbide polymer fiber precursor with uniform and stable quality. This embodiment employs a separator circulation type cooling medium conveyance passage structure.
Example 3
The silicon nitride polymer fiber precursor is collected in a net tray collecting device, the arrangement of the silicon nitride polymer fiber precursor is parallel to two sides of the net tray, and the diameter of the obtained silicon nitride polymer fiber precursor is 20 mu m by adjusting the collecting distance between the net tray and the filament making equipment and the concentration of the precursor. Firstly, placing a net tray collecting device for collecting silicon nitride polymer fiber precursors into a closed box body provided with a transmission window; secondly, the closed box body is vacuumized to ensure that the initial vacuum degree of the container is 6 multiplied by 10 -5 Pa, continuing for 4 hours under the initial vacuum degree, then injecting nitrogen to enable the pressure in the closed box body to be 500Pa, starting a cooling system, adopting helium as a medium, and enabling the flow speed to be 30m 3 /h; and finally, starting an electron beam irradiation system to irradiate the silicon nitride polymer fiber precursor for 70 minutes under the irradiation energy of 15MGy electron beams, so as to obtain the crosslinked cured silicon nitride polymer fiber precursor with uniform and stable quality. This embodiment employs a partition convergent cooling medium delivery passage structure.
Example 4
Collecting silicon nitride polymer fiber precursorIn the wire tray collecting device, the arrangement of the silicon nitride polymer fiber precursor forms an included angle of 30 degrees with one side of the wire tray, and the diameter of the obtained silicon nitride polymer fiber precursor is 18 mu m by adjusting the collecting distance between the wire tray and the wire making equipment and the concentration of the precursor. Firstly, placing a net tray collecting device for collecting silicon nitride polymer fiber precursors into a closed box body provided with a transmission window; secondly, vacuumizing the closed box body to ensure that the initial vacuum degree of the container is 10 -5 Pa, continuing for 3 hours under the initial vacuum degree, then injecting argon gas to ensure that the pressure in the closed box body is 30Pa, starting a cooling system, adopting high-temperature silicone oil as a medium, and ensuring that the flow speed is 20m 3 /h; and finally, starting an electron beam irradiation system to irradiate the silicon nitride polymer fiber precursor for 30min under the irradiation energy of the electron beam of 25MGy, so as to obtain the crosslinked cured silicon nitride polymer fiber precursor with uniform and stable quality. This embodiment employs a pipe circulation type cooling medium conveying passage structure.
Example 5
The silicon carbide polymer fiber precursor is collected in a net tray collecting device, the arrangement of the silicon carbide polymer fiber precursor is parallel to two sides of the net tray, and the diameter of the obtained silicon carbide polymer fiber precursor is 20 mu m by adjusting the collecting distance and the precursor concentration between the net tray and the filament making equipment. Firstly, placing a net tray collecting device for collecting silicon carbide polymer fiber precursors into a closed box body provided with a transmission window; secondly, the closed box body is vacuumized to ensure that the initial vacuum degree of the container is 5 multiplied by 10 -4 Pa, continuing for 5 hours under the initial vacuum degree, then injecting nitrogen to enable the pressure in the closed box body to be 1000Pa, starting a cooling system, adopting salt water as a medium, and enabling the flow speed to be 10m 3 /h; and finally, starting an electron beam irradiation system to irradiate the silicon carbide polymer fiber precursor for 20min under the irradiation energy of the 35MGy electron beam, so as to obtain the crosslinked cured silicon carbide polymer fiber precursor with uniform and stable quality. This embodiment employs a pipe circulation type cooling medium conveying passage structure.
Example 6
Collecting carbon fiber precursors in a net tray collecting device, arranging the carbon fiber precursors parallel to two sides of the net tray,the diameter of the obtained carbon fiber precursor was made 10 μm by adjusting the collection distance between the wire tray and the filament-making apparatus and the precursor concentration. Firstly, placing a net tray collecting device for collecting carbon fiber precursor into a closed box body provided with a transmission window; secondly, the closed box body is vacuumized to ensure that the initial vacuum degree of the container is 2 multiplied by 10 -4 Pa, continuing for 15 hours under the initial vacuum degree, then injecting argon gas to ensure that the pressure in the closed box body is 5000Pa, starting a cooling system, adopting air as a medium, and ensuring that the flow speed is 80m 3 /h; and finally, starting an electron beam irradiation system to irradiate the carbon fiber precursor for 60 minutes under the radiation energy of the 10MGy electron beam, so as to obtain the crosslinked and solidified carbon fiber precursor with uniform and stable quality. This embodiment employs a separator circulation type cooling medium conveyance passage structure.
In summary, the present application provides a method for crosslinking and curing inorganic fiber precursors, wherein the inorganic fiber precursors arranged in the same orientation are placed in a vacuum state, and then are placed in an inert gas atmosphere for electron beam irradiation, so as to obtain the crosslinked and cured inorganic fiber precursors. The application also designs an inorganic fiber precursor crosslinking curing device, which utilizes a net disk collecting device to ensure that fiber precursors are distributed in the same orientation, and compared with the traditional drum-type collecting device, the device can be more uniformly irradiated by electron beams; the introduction of the cooling system is beneficial to heat transmission and avoids the melting of the fiber precursor; the introduction of the vacuum system can avoid the influence of oxygen on the fiber precursor, and can effectively realize the rapid dissipation of heat, thereby further avoiding the melting of the fiber precursor. The method has spectrum adaptability, can realize the crosslinking and curing of the silicon carbide fiber precursor, the silicon nitride fiber precursor and the carbon fiber precursor, and can also be used for the crosslinking and curing of other inorganic fiber precursors. The method is simple and low in cost, and can effectively realize the rapid crosslinking and solidification of the inorganic fiber precursor before melting.
The present application has been described in connection with the most practical and preferred embodiments considered as presently to be understood, the foregoing description is not intended to limit the application to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, alternatives, and equivalents falling within the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. The inorganic fiber precursor crosslinking curing method is characterized by comprising the following steps of:
s1, arranging inorganic fiber precursors in the same orientation, wherein the inorganic fiber precursors are arranged in an orientation way through a net disc collecting device, and the inorganic fiber precursors are any one of silicon carbide fiber precursors, silicon nitride fiber precursors and carbon fiber precursors;
s2, placing the inorganic fiber precursor in the step S1 in a vacuum state, then placing the inorganic fiber precursor in an inert gas atmosphere, and simultaneously starting a cooling system;
and S3, irradiating the inorganic fiber precursor after the step S2 by using an electron beam to obtain the crosslinked and solidified inorganic fiber precursor.
2. The method for crosslinking and curing inorganic fiber filaments as claimed in claim 1, wherein in step S2, the degree of vacuum in the vacuum state is<10 -3 Pa, the inorganic fiber precursor is placed in the vacuum state for a time of at least 2 hours.
3. The method for crosslinking and curing inorganic fiber precursors according to claim 1, wherein in step S2, the vacuum degree of the inert gas atmosphere is maintained at 10Pa to 10Pa 4 Pa.
4. The method of crosslinking and curing inorganic fiber precursors according to claim 1, wherein in step S2, the inert gas is any one of nitrogen, argon and helium.
5. The method for crosslinking and curing inorganic fiber precursors according to claim 1, wherein in the step S3, the irradiation energy of the electron beam is 5 MGy-50 MGy, and the irradiation time is 5 min-80 min.
6. The method for crosslinking and curing inorganic fiber precursors according to claim 1, wherein the diameter of the inorganic fiber precursors is controlled to be 3 μm to 30 μm.
7. A device applied to the inorganic fiber precursor crosslinking and curing method as claimed in any one of claims 1 to 6, which is characterized by comprising an electron beam irradiation system (1), a closed box body (3) arranged under the electron beam irradiation system (1) and provided with a transmission window (2), and a net tray collecting device (5) arranged in the closed box body (3) and enabling inorganic fiber precursors (4) to be arranged in the same orientation, wherein a vacuumizing gas outlet (6) connected with a vacuum system and an inert gas inlet (7) for injecting inert gas are arranged on the closed box body (3), a cooling system for cooling the inorganic fiber precursors (4) is arranged on the outer side of the closed box body (3), and a monitoring device for monitoring the vacuum degree of the closed box body (3) in real time is also arranged.
8. An apparatus according to claim 7, characterized in that the vacuum system comprises a vacuum-pumping unit connected to the gas outlet (6) and an inert gas injection unit connected to the inert gas inlet (7).
9. Device according to claim 7, characterized in that the cooling system is realized by providing a sealed cooling jacket (8) on the outside of the closed box (3) in connection with a cooling medium inlet (9) and a cooling medium outlet (10).
10. The apparatus of the inorganic fiber filament cross-linking curing method as recited in claim 9, wherein the medium introduced at said cooling medium inlet (9) is any one of water, brine, alcohol-water mixture, oil, air, argon, helium, refrigerant.
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| CN201911329467.XA CN111005206B (en) | 2019-12-20 | 2019-12-20 | Inorganic fiber precursor crosslinking curing method and device |
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| CN201911329467.XA CN111005206B (en) | 2019-12-20 | 2019-12-20 | Inorganic fiber precursor crosslinking curing method and device |
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| CN111005206B true CN111005206B (en) | 2023-11-10 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN103046166A (en) * | 2013-01-25 | 2013-04-17 | 中国人民解放军国防科学技术大学 | Chemical gas-phase crosslinking method of polycarbosilane fibers |
| CN106637915A (en) * | 2016-12-01 | 2017-05-10 | 中国人民解放军国防科学技术大学 | Auxiliary gas-phase cross-linking method of electron beams |
| CN106757530A (en) * | 2017-01-22 | 2017-05-31 | 中国科学院过程工程研究所 | Electron beam irradiation crosslinking prepares the method and device of BN fibers |
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