CN112304095A - Ultra-high temperature sintering furnace - Google Patents
Ultra-high temperature sintering furnace Download PDFInfo
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- CN112304095A CN112304095A CN202011189313.8A CN202011189313A CN112304095A CN 112304095 A CN112304095 A CN 112304095A CN 202011189313 A CN202011189313 A CN 202011189313A CN 112304095 A CN112304095 A CN 112304095A
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- 238000005245 sintering Methods 0.000 title claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 100
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000009529 body temperature measurement Methods 0.000 claims abstract description 14
- 230000005484 gravity Effects 0.000 claims abstract description 13
- 238000009413 insulation Methods 0.000 claims abstract description 12
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- 230000006698 induction Effects 0.000 claims description 23
- 229910002804 graphite Inorganic materials 0.000 claims description 22
- 239000010439 graphite Substances 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 8
- 238000012544 monitoring process Methods 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 238000005452 bending Methods 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000000462 isostatic pressing Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 230000002457 bidirectional effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000011161 development Methods 0.000 abstract description 4
- 229920000049 Carbon (fiber) Polymers 0.000 description 10
- 239000004917 carbon fiber Substances 0.000 description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 238000005087 graphitization Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000009991 scouring Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical class S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 229910052815 sulfur oxide Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D11/00—Arrangement of elements for electric heating in or on furnaces
- F27D11/02—Ohmic resistance heating
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D11/00—Arrangement of elements for electric heating in or on furnaces
- F27D11/06—Induction heating, i.e. in which the material being heated, or its container or elements embodied therein, form the secondary of a transformer
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D19/00—Arrangements of controlling devices
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D21/00—Arrangements of monitoring devices; Arrangements of safety devices
- F27D21/0014—Devices for monitoring temperature
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
- F27D2007/063—Special atmospheres, e.g. high pressure atmospheres
Abstract
The invention belongs to the technical field of ultra-high temperature vacuum, and particularly relates to an ultra-high temperature sintering furnace. Can improve the production efficiency, reduce the production cost, break through the bottleneck of the prior art in China and meet the requirement of industrial development. Comprises a furnace body, a furnace door, a vacuum system and a heating chamber; the vacuum furnace is characterized in that an evacuation interface of the vacuum system is communicated with a furnace body cavity; the heating chamber is arranged in the furnace body cavity; the heating chamber comprises a resistance-type heating chamber or an induction-type heating chamber, heating bodies and heat insulation layers are arranged in the two heating chambers, and the heating bodies are arranged in the heat insulation layers; the top of the furnace body is provided with a low-temperature thermocouple assembly, an infrared temperature measurement assembly and a gravity valve; argon is filled into the furnace in a large flow mode by adopting a metal rotor flow meter at the low-temperature section, and argon is continuously filled into the furnace in a small flow mode by adopting a mass flow meter at the high-temperature section; the furnace body is provided with a gravity valve, and the working port of the gravity valve is communicated with the working cavity of the furnace body.
Description
Technical Field
The invention belongs to the technical field of ultra-high temperature vacuum, and particularly relates to an ultra-high temperature sintering furnace, in particular to an ultra-high temperature sintering furnace at 3000 ℃.
Background
With the rapid development of chemical, mechanical, building, metallurgy, nuclear power, and in particular aerospace industries, carbon fiber is widely used in various fields as a new generation of structural and functional materials with superior properties, such as high strength, high modulus, low density, low expansion, high temperature resistance, friction resistance, impact resistance, corrosion resistance, fatigue resistance, self lubrication, heat conduction, and electrical conduction, which are incomparable to other materials, and has attracted general attention of researchers.
The main purpose of the carbon fiber graphitization treatment is to induce fiber graphitization crystal orientation to increase the elastic modulus of the carbon fiber. A large number of researches prove that the tensile modulus of the carbon fiber is improved along with the increase of the graphitization temperature, so that high-temperature technology and high-temperature equipment are required for producing the carbon fiber, the technical content is high, the conditions are harsh, in addition, the core technology is difficult to introduce, the countries for the industrial production of the high-performance graphite fiber and the formation of series products are Japan and America, and China cannot form large-scale production so far. The existing high-temperature sintering furnace in China can not realize uniform heating at 3000 ℃, the technical difficulty is difficult to break through, the graphitization degree of the carbon fiber is low, the tensile modulus is far lower than the theoretical upper limit, and the carbon fiber with higher modulus can not be prepared. Meanwhile, the phenomena of difficult control of the temperature of large workpieces, large temperature uniformity deviation and high energy consumption generally occur, and the development and application of the products are severely restricted.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the 3000 ℃ ultra-high temperature sintering furnace, which can produce high-strength and high-modulus carbon fiber products, not only reduces heat loss and obtains high furnace temperature uniformity, but also can improve production efficiency, reduce production cost, break through the bottleneck of the prior art in China and meet the needs of industrial development.
In order to achieve the purpose, the invention adopts the following technical scheme that the furnace comprises a furnace body, a furnace door, a vacuum system and a heating chamber; it is characterized in that the evacuation interface of the vacuum system is communicated with the furnace body cavity.
The heating chamber is arranged in the furnace body cavity.
The heating chamber comprises a resistance-type heating chamber or an induction-type heating chamber, heating bodies and heat preservation layers are arranged in the two heating chambers, and the heating bodies are arranged in the heat preservation layers.
The top of the furnace body is provided with a low-temperature thermocouple assembly, an infrared temperature measurement assembly and a gravity valve.
The low-temperature section adopts a metal rotor flow meter to fill the (high-purity) argon into the furnace in a large flow mode, and the high-temperature section adopts a (high-precision) mass flow meter to continuously fill the argon into the furnace in a small flow mode.
The furnace body is provided with a gravity valve, and the working port of the gravity valve is communicated with the working cavity of the furnace body.
Furthermore, the heating body is connected with the output end of the power supply system through an electrode.
Furthermore, the right side of the furnace body is connected with an inflation and deflation system, and the working port of the inflation and deflation system is communicated with the working cavity of the furnace body. So as to realize temperature measurement, inflation and overpressure protection in vacuum, negative pressure and micro-positive pressure environments.
Furthermore, in the resistance-type heating chamber, the heating body comprises a heating element which is arranged in a multi-zone or single-zone manner, and the heating element is formed by connecting isostatic pressing graphite threads; the heat-insulating layer is of a two-layer layered structure and comprises an inner-layer hard felt and an outer-layer soft graphite felt; the heat preservation holds in the frame, and the frame is fixed in the furnace body inner wall through the connecting plate, sets up electrode lead-out hole, low temperature thermocouple subassembly hole, infrared temperature measurement subassembly hole, exhaust hole and heat preservation fixed orifices on the frame.
Further, the outer contour of the heating body is one of a rod-shaped square frame, a strip-shaped square frame or an arc-shaped circular ring, and is connected with the electrode through a gas insulation structure.
Further, in the induction heating chamber: the heating body is assembled into a rectangular chamber or a round chamber by graphite, and the heat insulation layer is composed of soft graphite felt; the induction heating chamber also comprises an inductor, the inductor is a rectangular frame induction coil or a round cylinder induction coil which is formed by bending a rectangular copper tube, the induction coils are connected in parallel in a single group or multiple groups, the outer wall of the inductor is sprayed by ceramic, the inductor is fixed in an outer frame, and the outer frame of the inductor is fixed on the inner wall of the furnace body through a connecting plate.
Furthermore, the furnace body and the furnace door are of sandwich structures, and the sandwich layer of the sandwich structure is hollow; and a bidirectional sealing structure is arranged between the furnace body and the furnace door.
Further, a bearing hearth is arranged in the heating body, and the bearing hearth comprises a multi-point support piece.
Further, the multi-point support is machined from graphite.
Furthermore, the low-temperature thermocouple assembly is a plug-in thermocouple, and a monitoring thermocouple is arranged outside the heat insulation layer.
Compared with the prior art, the invention has the beneficial effects.
The heating chamber structure form I (resistance heating chamber) of the invention: the heating body can be designed into multi-region or single-region arrangement, and the structural form can be designed into a square frame, a polygon or a circle according to the shapes of the furnace shell and the temperature region, so that the structure is compact and the energy consumption is low; the heating element can be designed in a rod shape, a plate shape or an arc shape; the thermal field structure design provides an optimal hot area for sintering materials, further ensures high temperature uniformity and greatly improves the product quality.
The heating chamber structure form II (induction heating chamber) of the invention: the heating chamber can be designed into a single-group or multi-group parallel inductor structure, the induction coils are bent into a rectangular frame or a round cylinder according to structural arrangement, multi-path cooling water is convenient to introduce by grouping design, the cooling effect of the induction coils is ensured, the thermal shock influence of the coils in a high-temperature environment is effectively protected, and meanwhile, the induction of a magnetic field at the power feeding part to the side flange of the furnace body is reduced by the multi-group incoming wires.
The heat-insulating layer of the invention consists of a soft graphite felt and a graphite plate (or a hard felt), adopts a heat-insulating material with lower heat conductivity, improves the heating power, enables the temperature of the furnace core to reach the required highest temperature as soon as possible, and reduces the heat radiation of the furnace. The smooth surface of the graphite plate (or the hard felt) has good corrosion resistance and airflow scouring effect, the high-temperature service life of the heating chamber is prolonged, and the cost is effectively saved.
In order to ensure that the pressure is controllable under the ultra-high temperature environment of 3000 ℃, a metal rotor flow meter is adopted to charge air into the furnace in a large flow mode at the low-temperature section, and a mass flow meter is adopted to achieve dynamic balance in the whole sintering process in a small flow mode at the high-temperature section, so that the pressure and the air flow field are stable, the workpiece is sintered uniformly, the working efficiency is effectively improved, and the air consumption is reduced.
When the temperature in the furnace reaches 3000 ℃ ultra-high temperature environment, the over-high air pressure in the hearth is automatically discharged through the gravity valve, so that the over-pressure is avoided.
The monitoring couple is arranged outside the heat-insulating layer, so that the equipment is prevented from being damaged due to failure of the heat-insulating layer, necessary protection is a powerful guarantee for continuous and stable production of the ultra-high temperature equipment, and the monitoring value has an early warning effect on the maintenance period of the heating chamber.
The invention adopts advanced temperature measurement and control technology, has the characteristics of large capacity, quick temperature rise, high temperature, and sensitive and accurate temperature measurement and control, and can be used for high-temperature graphitization treatment of other carbon products, and high-temperature sintering and heat treatment of metal powder.
Drawings
The invention is further described with reference to the following figures and detailed description. The scope of the invention is not limited to the following expressions.
Fig. 1 is a schematic view of the overall structure of the present invention.
FIG. 2 is a top view of the present invention.
FIG. 3 is a schematic view of a heating chamber according to the present invention.
FIG. 4 is a schematic view of a second embodiment of the heating chamber of the present invention.
Detailed Description
As shown in fig. 1, 2, 3 and 4, the 3000 ℃ ultra-high temperature sintering furnace comprises a furnace body 1, a furnace door 2, a vacuum system 3, a heating chamber 4, an electrode 5, a low temperature thermocouple assembly 6, an infrared temperature measurement assembly 7, a gravity valve 8, a charging and discharging system 9 and a power supply system 10. And the evacuation interface of the vacuum system 3 is communicated with the cavity of the furnace body 1.
The heating chamber 4 is arranged in the cavity of the furnace body 1; the heating chamber 4 comprises two heating modes of resistance and induction, and a heating body 403/407 is arranged in the heating chamber; the heating element 403/407 is arranged on the inner side of the heat-insulating layer 402; the heating element 403/407 is connected with the output end of the power supply system 10 through the electrode 5; the low-temperature thermocouple assembly 6, the infrared temperature measurement assembly 7 and the gravity valve 8 are arranged at the top of the furnace body 1, the interface of the inflation and deflation system 9 is arranged at the right side of the furnace body 1, and the working port of the inflation and deflation system is communicated with the working cavity of the furnace body 1, so that temperature measurement, inflation and overpressure protection in vacuum, negative pressure and micro-positive pressure environments are realized.
As shown in fig. 3, the heating chamber 4 of the present invention has a first structure (resistance heating chamber): comprises a heating body 403, a heat-insulating layer 402, a frame 401 and a bearing hearth 404; the heating unit 403 comprises heating elements arranged in multiple zones or single zone, and is made of an inlet isostatic pressing graphite material; the heating body 403 can be designed into a rod-shaped frame according to the shape of the heating chamber 4, if the frame body of the heating chamber 4 is polygonal, the heating body 403 can be correspondingly designed into a polygonal frame, and if the heating chamber 4 is circular, the heating body 403 can be correspondingly designed into an arc-shaped ring; the heating body 403 is connected with an electrode 5 by a special insulating structure, and the electrode 5 is connected with a power supply system 10 (thyristor voltage-regulating power supply); each zone is provided with an independently adjustable heating element, and the zones form a controllable uniform temperature field, so that the product quality is greatly improved; the heat insulation layer 402 is formed by compounding a hard felt 4021 and a soft graphite felt 4022; the soft graphite felt 4022 is a high-quality felt which is treated at high temperature and has low ash content; an electrode 5 leading-out hole, a low-temperature thermocouple assembly 6 hole, an infrared temperature measurement assembly 7 hole, an exhaust hole and an insulating layer 402 fixing hole are formed in the frame 401 and are fixed on the inner wall of the furnace body 1 through a connecting plate 405.
As shown in fig. 4, the second structural form of the heating chamber 4 (induction heating chamber) of the present invention: comprises a heating body 407, an insulating layer 402, an inductor 406 and a bearing hearth 404; the heating body 407 is a rectangular or circular chamber assembled by high-quality graphite and is arranged inside the heat-insulating layer 402; the heat preservation layer 402 is composed of a soft graphite felt 4022, the inductor 406 is a rectangular frame or a circular cylinder formed by bending a rectangular copper tube, induction coils are designed into a single group or multiple groups to be connected in parallel according to structural arrangement requirements, multi-path cooling water is convenient to introduce by group design, the cooling effect of the induction coils is ensured, the thermal shock influence of the coils in a high-temperature environment is effectively protected, and meanwhile, the induction of a magnetic field at an electric inlet part to a flange at the side of the furnace body 1 is reduced by multiple groups of inlet wires; the power supply system 10 (medium frequency induction power supply) is connected through a copper bar, and alternating current is led into a connector of the inductor 406; the outer wall of the inductor 406 is insulated with ceramic, and the outer frame thereof is fixed to the inner wall of the furnace body 1 through a connecting plate 405.
As shown in fig. 3, the heat insulating layer 402 of the present invention is formed by combining a hard felt 4021 and a soft graphite felt 4022; as shown in fig. 4, the inventive insulation 402 is comprised of a soft graphite felt 4022. The graphite plate or the hard felt 4021 has a smooth surface, is resistant to corrosion and has a good air flow scouring effect, the high-temperature service life of the heating chamber 4 is prolonged, and the cost is effectively saved.
As shown in FIG. 1, the temperature measuring device of the invention is composed of a low-temperature thermocouple assembly 6 and an infrared temperature measuring assembly 7; the low-temperature thermocouple assembly 6 is driven by a cylinder, lowers the thermocouple into the heating chamber 4, and measures a low-temperature region (0-1200 ℃); when the temperature exceeds 1200 ℃, the thermocouple is automatically lifted, the infrared temperature measurement component 7 starts to work, and the temperature of the high-temperature area (1200-.
As shown in fig. 2, the inflation and deflation system 9 comprises an inflation valve, a flow control system, a pressure gauge, a pipeline, a joint and the like; and the signal transmission port of the flow control system is connected with an execution control port of the inflation and deflation system 9 and is used for meeting the inflation requirement required by the process. In order to ensure that the pressure is controllable under the ultra-high temperature environment of 3000 ℃, a metal rotor flow meter is adopted to charge gas into the furnace in a large flow mode at the low-temperature section, and a mass flow meter is adopted to achieve dynamic balance in the whole sintering process in a small flow mode at the high-temperature section, so that the pressure and gas flow field are stable, the workpiece is sintered uniformly, the working efficiency is effectively improved, and the gas consumption is reduced.
As shown in figure 1, when the temperature in the furnace reaches 3000 ℃ ultra-high temperature environment, the over-high air pressure in the furnace body 1 is automatically discharged through the gravity valve 8, so as to avoid over-pressure.
As shown in fig. 3 and 4, a monitoring couple is arranged outside the insulating layer 402 to prevent the insulating layer 402 from failing and damaging equipment, necessary protection is a powerful guarantee for stable production of the ultra-high temperature equipment, and the monitoring value has an early warning effect on the maintenance period of the heating chamber 4.
As shown in figure 2, the furnace body 1 of the invention adopts a horizontal structure, the power supply system 10 is arranged at the rear side of the furnace body 1, the whole layout is compact and reasonable, the operation and maintenance are convenient, and the whole equipment is above the ground.
The working principle of the invention is as follows.
The method comprises the steps of firstly, loading the carbon material to be sintered into a sintering furnace, vacuumizing in advance and repeatedly flushing with high-purity argon before heating is started, removing oxygen adsorbed in the heating element 403/407 and the heat-insulating layer 402 as far as possible, and when the degree of vacuum in the furnace reaches the required degree, feeding power to the power supply system 10 and then heating the heating element 403/407. The low-temperature thermocouple assembly 6 is driven by a cylinder, a thermocouple is lowered into the heating chamber 4, and a low-temperature region (0-1200 ℃) is measured; when the temperature exceeds 1200 ℃, the thermocouple is automatically lifted, the infrared temperature measurement component 7 starts to work, and the temperature of the high-temperature area (1200-. Because the carbon fiber material has higher sintering temperature, the sintering is generally carried out at the high temperature of 2200-. The first embodiment is as follows: the resistance heating is that the electrode 5 directly acts on the heating body 403, the graphite is heated by the heat effect of the current, the temperature of each area is adjustable, the temperature uniformity is good, and the deformation and the thermal shock of the sintering material are small; example two: in the induction heating, magnetic lines of force generated by the induction current are concentrated on the heating element 407, and eddy current is generated by the induction action of the electromagnetism to heat the heating element 407. The whole sintering temperature rise process can generate redundant gases such as hydrogen sulfide, sulfur oxides, carbon monoxide, carbon dioxide and the like, so that the gases are discharged out of the furnace to a washing tower through gas flow under a micro-positive pressure environment. Meanwhile, the 3000 ℃ sintering process is accompanied by oxidation consumption and high-temperature sublimation loss phenomena, so that the service life of the heating element 403/407 is shortened, and high-purity inert gas is introduced in the heating process to realize positive-pressure sealing heating of protective gas so as to reduce element evaporation. And finally, after heat preservation is carried out for 10-20 hours, stopping heating, and when the temperature in the furnace is cooled to a set temperature, taking materials out of the furnace to finish the whole sintering process, thereby obtaining a high-strength and high-modulus high-quality carbon fiber product.
It should be understood that the detailed description of the present invention is only for illustrating the present invention and is not limited by the technical solutions described in the embodiments of the present invention, and those skilled in the art should understand that the present invention can be modified or substituted equally to achieve the same technical effects; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (10)
1. An ultra-high temperature sintering furnace comprises a furnace body, a furnace door, a vacuum system and a heating chamber; the vacuum furnace is characterized in that an evacuation interface of the vacuum system is communicated with a furnace body cavity;
the heating chamber is arranged in the furnace body cavity;
the heating chamber comprises a resistance-type heating chamber or an induction-type heating chamber, heating bodies and heat insulation layers are arranged in the two heating chambers, and the heating bodies are arranged in the heat insulation layers;
the top of the furnace body is provided with a low-temperature thermocouple assembly, an infrared temperature measurement assembly and a gravity valve;
argon is filled into the furnace in a large flow mode by adopting a metal rotor flow meter at the low-temperature section, and argon is continuously filled into the furnace in a small flow mode by adopting a mass flow meter at the high-temperature section;
the furnace body is provided with a gravity valve, and the working port of the gravity valve is communicated with the working cavity of the furnace body.
2. The ultra-high temperature sintering furnace according to claim 1, characterized in that: the heating body is connected with the output end of the power supply system through the electrode.
3. The ultra-high temperature sintering furnace according to claim 1, characterized in that: the right side of the furnace body is connected with an inflation and deflation system, and the working port of the inflation and deflation system is communicated with the working cavity of the furnace body.
4. The ultra-high temperature sintering furnace according to claim 1, characterized in that: in the resistance-type heating chamber, the heating body comprises a heating element which is arranged in a plurality of areas or a single area, and the heating element is formed by connecting isostatic pressing graphite threads; the heat-insulating layer is of a two-layer layered structure and comprises an inner-layer hard felt and an outer-layer soft graphite felt; the heat preservation holds in the frame, and the frame is fixed in the furnace body inner wall through the connecting plate, sets up electrode lead-out hole, low temperature thermocouple subassembly hole, infrared temperature measurement subassembly hole, exhaust hole and heat preservation fixed orifices on the frame.
5. The ultra-high temperature sintering furnace according to claim 4, characterized in that: the outer contour of the heating body is one of a rod-shaped square frame, a strip-shaped square frame or an arc-shaped circular ring, and is connected with the electrode through a gas insulation structure.
6. The ultra-high temperature sintering furnace according to claim 1, characterized in that: in the induction heating chamber: the heating body is assembled into a rectangular chamber or a round chamber by graphite, and the heat insulation layer is composed of soft graphite felt; the induction heating chamber also comprises an inductor, the inductor is a rectangular frame induction coil or a round cylinder induction coil which is formed by bending a rectangular copper tube, the induction coils are connected in parallel in a single group or multiple groups, the outer wall of the inductor is sprayed by ceramic, the inductor is fixed in an outer frame, and the outer frame of the inductor is fixed on the inner wall of the furnace body through a connecting plate.
7. The ultra-high temperature sintering furnace according to claim 1, characterized in that: the furnace body and the furnace door are of sandwich structures, and the sandwich layer of the sandwich structure is hollow; and a bidirectional sealing structure is arranged between the furnace body and the furnace door.
8. The ultra-high temperature sintering furnace according to claim 1, characterized in that: a bearing hearth is arranged in the heating body and comprises a multi-point support piece.
9. The ultra-high temperature sintering furnace according to claim 8, characterized in that: the multipoint support member is machined from graphite.
10. The ultra-high temperature sintering furnace according to claim 1, characterized in that: the low-temperature thermocouple assembly is a plug-in thermocouple, and a monitoring thermocouple is arranged outside the heat insulation layer.
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| CN113847805A (en) * | 2021-09-28 | 2021-12-28 | 山东交通学院 | Ultra-high temperature sintering furnace |
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