CN100546944C - The technology of the long-pending preparation of electric heating process orienting infiltration charcoal/charcoal component - Google Patents
The technology of the long-pending preparation of electric heating process orienting infiltration charcoal/charcoal component Download PDFInfo
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Abstract
The present invention relates to the technology of the long-pending preparation of a kind of electric heating process orienting infiltration charcoal/charcoal component, this technology comprises three partial contents: the design of electric heating process CVI cvd furnace; The preparation of precast body; The densification of precast body and high-temperature heat treatment.Specifically be that precast body self directly is used as heating element, as the electrode of power supply, add electric current at the two ends of precast body in cvd furnace, the self-resistance generation heat by precast body reaches more than the pyrolysis temperature of reactant gases furnace chamber.
Description
(1) technical field:
The invention provides the technology of the long-pending preparation of electric heating process orienting infiltration charcoal/charcoal component, belong to the carbon/carbon composite technical field.
(2) background technology:
Charcoal/charcoal (C/C) matrix material has high specific strength and specific modulus under hot environment, low density and good anti-ablation, hot physics, mechanical behavior under high temperature, particularly they can keep very reasonably frictional coefficient in very big range of temperature, be successfully used to the guided missile nose cone of strategic nuclear weapons, the jet pipe throat lining of rocket engine, the nose cone of space shuttle and military affairs such as the leading edge of a wing and aeroplane brake discs, aerospace field, but this material causes cost very high because the price of charcoal fiber raw material is high and preparation technology's cycle is long, so far they also do not obtain widespread use in industry and the civilian field of waiting, and therefore research and develop fast and low-cost densification new technology and be one of key subjects that present international C/C matrix material studies.
Aspect the densification of C/C matrix material, main both at home and abroad at present resin method and long-pending (CVI) method of chemical vapor infiltration of adopting.Resin method generally needs repeatedly circulation to immerse resin or pitch carries out charing and greying then, isothermal CVI method precast body then needs densification more than 1000 hours, these caused the C/C Composite Preparation cycle long, cost is high, and greatly limited its range of application, thereby a large amount of manpower and materials research quick densifying technology have all been dropped into both at home and abroad, thermal gradient CVI, novel procesies such as forced convection thermal gradient CVI, directly-heated CVI have been proposed in succession, but these methods for various reasons, all do not obtain big application in industry.
Electric heating process (electrified perform heating CVI method, be called for short ECVI) be by to temperature, pressure, contact area and free space volumes than isoparametric control, the residence time of pilot-gas, it is long-pending to realize that deposit carbon successively oozes to outside disposable from precast body inside, make the long-pending speed of oozing of carbon improve an order of magnitude, reduce the densification cost greatly.In conjunction with to RESEARCH OF PYROCARBON type, weave construction, Interface Design, improve mechanical property, tribological property and material self resistance of oxidation simultaneously, for good basis is established in the actual application of C/C matrix material (particularly using as aeroplane brake discs).
(3) summary of the invention:
The object of the present invention is to provide the technology of the long-pending preparation of a kind of electric heating process orienting infiltration charcoal/charcoal component, solve long, defect of high cost of C/C Composite Preparation cycle in the prior art, prepare fast have strong mechanical performance, the C/C matrix material of good heat physical properties, to reduce cost.
The technology of the long-pending preparation of a kind of electric heating process orienting infiltration of the present invention charcoal/charcoal component, its technical scheme is divided into following a few part: the preparation of precast body, the design of electric heating process CVI cvd furnace, the densification of precast body and high-temperature heat treatment; Its technical process is as shown in Figure 1:
1. the preparation of precast body
At first, adopt whole Nomex as precast body, its structural unit is one deck net tire+two-layer no latitude cloth, and the macrofiber between two layers of no latitude cloth adopts quadrature (90 °) shop layer, lays evenly; The shop number of plies should be not less than 15 layers; No latitude cloth adopts the T300PAN based carbon fiber, and the ratio that its weight accounts for overall weight is 〉=75%; The net tire also adopts the T300PAN based carbon fiber, and its weight ratio is≤25%; Initial density is 0.5g/cm
3About.Then, the Nomex precast body is fixed on the homemade graphite anchor clamps, in the groove of graphite body, precast body is fixed.These graphite anchor clamps mainly are made up of graphite body and isolator two parts, two of the bottom independently graphite body and two copper electrodes be spirally connected fixingly respectively, the graphite body at top is by the isolator fixed support, as shown in Figure 2.
2. electric heating process CVI cvd furnace design
Electric heating process CVI cvd furnace as shown in Figure 3.Electrical insulator and two copper electrodes are installed in the bottom of body of heater, the inwall of body of heater is installed cooling system, and be provided with thermofin and avoid the furnace body outer wall temperature too high, but viewport has been installed on the body of heater, be used to observe the intravital various phenomenons of stove, inlet mouth is installed in the bottom of body of heater, the air outlet is installed in the top of body of heater, precast body is fixed in the graphite anchor clamps of being made by graphite body, the isolator fixed support graphite body of body of heater center, and cooling system is installed at the center of isolator, thermocouple is installed on the precast body surface, be used to measure the temperature on precast body surface, thermocouple is installed on the precast body centre portions, is used to measure the temperature of precast body centre portions.
3. the densification of precast body and high-temperature heat treatment
At first vacuumize to check and whether leak gas, feed nitrogen then and purify body of heater, continue to feed nitrogen and reach a normal atmosphere up to the intravital air pressure of stove; Then precast body being heated to surface temperature is 700～800 ℃, will continue to feed nitrogen simultaneously, and the effect of nitrogen is to prevent the precast body oxidation.The temperature of the temperature of precast body outside surface and inside center part utilizes two thermocouple to test, and one is fixed on the precast body surface, and another is fixed on precast body central part office.When the temperature at center reaches 900～1100 ℃, feed the mixed gas of Sweet natural gas and nitrogen.Carry out along with sedimentary, the temperature that measures in the thermocouple of surface portion can slowly rise, and levels off to the temperature at precast body center, but depositing temperature still remains on 900～1100 ℃ in whole deposition process, depositing time 80 hours, the precast body densification finishes; Then, the material through densification is carried out high-temperature heat treatment: material is placed in the vacuum carburization stove, under the state of nitrogen or argon shield, with the temperature rise rate of 30～50 ℃/h, is warmed up to 2000-2500 ℃, and is incubated 3～5 hours, get product.
Wherein, self directly is used as heating element this precast body, in cvd furnace as the electrode of power supply.
Wherein, add electric current, by the self-resistance generation heat of precast body at the two ends of this precast body.
Wherein, these graphite anchor clamps mainly are made up of graphite body and isolator two parts, two of the bottom independently graphite body and two copper electrodes be spirally connected fixingly respectively, the graphite body at top is by the isolator fixed support.
Wherein, the flow velocity of the gas mixture of feeding Sweet natural gas and nitrogen is 351/min.
Wherein, vacuumize to check that the speed that should guarantee to leak gas is less than 0.13Pa/min in the step of whether leaking gas at this
The technology of the long-pending preparation of a kind of electric heating process orienting infiltration of the present invention charcoal/charcoal component, its advantage and effect are:, the preparation cycle length of charcoal/charcoal component, cost are low, and the charcoal/charcoal component of preparing has strong mechanical performance, good heat physical properties.
(4) description of drawings:
The process flow sheet of the long-pending preparation of Fig. 1 electric heating process orienting infiltration charcoal/charcoal component
The homemade graphite anchor clamps of Fig. 2 synoptic diagram
Fig. 3 electric heating process CVI cvd furnace synoptic diagram
Concrete label and symbol are as follows:
1, air outlet 2, isolator 3, cooling system
4, thermocouple 5, graphite body 6, electrical insulator
But 7, copper electrode 8, precast body 9 viewports
10, thermocouple 11, cooling system 12, thermofin
13, inlet mouth
° degree, ℃ degree centigrade, ℃/h degree centigrade/hour,
The Pa/min handkerchief/minute, the 1/min liter/minute
(5) embodiment:
The technology of the long-pending preparation of a kind of electric heating process orienting infiltration of the present invention charcoal/charcoal component, its embodiment is described below in conjunction with the accompanying drawings:
1. the preparation of precast body
At first, adopt whole Nomex as precast body, precast body is of a size of 1100 * 500 * 35mm, and the volume content of charcoal fiber is 40%.Its structural unit is one deck net tire+two-layer no latitude cloth, and the macrofiber between two layers of no latitude cloth adopts quadrature (90 °) shop layer, lays evenly; The shop number of plies should be not less than 15 layers; No latitude cloth adopts the T300PAN based carbon fiber, and the ratio that its weight accounts for overall weight is 〉=75%; The net tire also adopts the T300PAN based carbon fiber, and its weight ratio is≤25%; Initial density is 0.5g/cm
3About.Then, the Nomex precast body is fixed on the homemade graphite anchor clamps, in the groove of graphite body, precast body is fixed.These graphite anchor clamps mainly are made up of graphite body 5 and isolator 2 two partss, two of the bottom independently graphite body 5 be and two copper electrodes 7 fixed that is spirally connected respectively that the graphite body at top is by isolator 2 fixed supports, as shown in Figure 2.
2. electric heating process CVI cvd furnace design
Electric heating process CVI cvd furnace as shown in Figure 3.Electrical insulator 6 and two copper electrodes 7 are installed in the bottom of body of heater, the inwall of body of heater is installed cooling system 11, and be provided with thermofin 12 and avoid the furnace body outer wall temperature too high, but viewport 9 has been installed on the body of heater, be used to observe the intravital various phenomenons of stove, inlet mouth 13 is installed in the bottom of body of heater, air outlet 1 is installed in the top of body of heater, precast body 8 is fixed in the graphite anchor clamps of being made by graphite body 5, the isolator 2 fixed support graphite bodies 5 of body of heater center, cooling system 3 is installed at the center of isolator 2, thermocouple 4 is installed on the precast body surface, be used to measure the temperature on precast body surface, thermocouple 10 is installed on the precast body centre portions, is used to measure the temperature of precast body centre portions.
3. the densification of precast body
Electric heating process CVI cvd furnace as shown in Figure 3, as presoma, the gas flow amount is 351/min with Sweet natural gas.Whether the first step of experiment is depositing device to be vacuumized inspection leak gas; The speed that guarantees to leak gas feeds nitrogen and purified body of heater in about 30 minutes less than 0.13Pa/min, feeds nitrogen then and reaches a normal atmosphere up to the intravital air pressure of stove.Then heat precast body; the temperature of the temperature of its outside surface and inside center part utilizes two thermocouple to test; a thermocouple is fixed on the precast body surface; another is fixed on the central part office of precast body thickness; control precast body core temperature is 900～1100 ℃, and surface temperature is 700～800 ℃, makes that thermograde is 200～300 ℃; will continue to feed nitrogen simultaneously, the effect of nitrogen is the anti-oxidation that plays a protective role.By the time after depositing temperature had been stablized 30 minutes, the mixed gas of Sweet natural gas and nitrogen fed in the cvd furnace.Carry out along with sedimentary; the temperature that measures in the thermocouple of surface portion can slowly rise, and levels off to the temperature at precast body center, but depositing temperature still remains on 900～1100 ℃ in whole deposition process; treat that depositing time reaches 80 hours; the precast body densification finishes, and then the material through densification is carried out high-temperature heat treatment: material is placed in the vacuum carburization stove, under the state of nitrogen protection; temperature rise rate with 30 ℃/h; be warmed up to 2500 ℃, and be incubated 3 hours, get product.
Claims (5)
1, the technology of the long-pending preparation of a kind of electric heating process orienting infiltration charcoal/charcoal component, it is characterized in that: its preparation technology is:
(1) preparation of precast body
At first, adopt whole Nomex as precast body, its structural unit is one deck net tire+two-layer no latitude cloth, and the macrofiber between the two-layer no latitude cloth adopts quadrature shop layer, lays evenly; The shop number of plies should be not less than 15 layers; No latitude cloth adopts T300 PAN based carbon fiber, and the ratio that its weight accounts for overall weight is 〉=75%; The net tire also adopts T300 PAN based carbon fiber, and its weight ratio is≤25%; Initial density is 0.5g/cm
3About; Then, the Nomex precast body is fixed on the homemade graphite anchor clamps, in the groove of graphite body, precast body is fixed;
Described homemade graphite anchor clamps mainly are made up of graphite body and isolator two parts, two of the bottom independently graphite body and two copper electrodes be spirally connected fixingly respectively, the graphite body at top is by the isolator fixed support;
(2) the long-pending cvd furnace design of electric heating process chemical vapor infiltration
Electrical insulator and two copper electrodes are installed in the bottom of body of heater, the inwall of body of heater is installed cooling system, and be provided with thermofin and avoid the furnace body outer wall temperature too high, but viewport is installed on the body of heater, be used to observe the intravital various phenomenons of stove, inlet mouth is installed in the bottom of body of heater, the air outlet is installed in the top of body of heater, precast body is fixed in the graphite anchor clamps of being made by graphite body, the isolator fixed support graphite body of body of heater center, and cooling system is installed at the center of isolator, a thermocouple is installed on the precast body surface, be used to measure the temperature on precast body surface, another thermocouple is installed on the precast body centre portions, is used to measure the temperature of precast body centre portions;
(3) densification of precast body and high-temperature heat treatment
At first vacuumize to check and whether leak gas, feed nitrogen then and purify body of heater, continue to feed nitrogen and reach a normal atmosphere up to the intravital air pressure of stove; Then precast body being heated to surface temperature is 700～800 ℃, will continue to feed nitrogen simultaneously; The temperature of the temperature of precast body outside surface and inside center part utilizes two thermocouple to test, and one is fixed on the precast body surface, and another is fixed on precast body central part office; When the temperature at center reaches 900～1100 ℃, feed the mixed gas of Sweet natural gas and nitrogen; Carry out along with sedimentary, the temperature that measures in the thermocouple of surface portion can slowly rise, and levels off to the temperature at precast body center; Depositing temperature remains on 900～1100 ℃ in the whole deposition process, depositing time 80 hours, and the precast body densification finishes; Then, the material through densification is carried out high-temperature heat treatment: material is placed in the vacuum carburization stove, under the state of nitrogen or argon shield, with the temperature rise rate of 30～50 ℃/h, is warmed up to 2000-2500 ℃, and is incubated 3～5 hours, get product.
2, the technology of the long-pending preparation of electric heating process orienting infiltration according to claim 1 charcoal/charcoal component, it is characterized in that: self directly is used as heating element this precast body, in cvd furnace as the electrode of power supply.
3, the technology of the long-pending preparation of electric heating process orienting infiltration according to claim 1 charcoal/charcoal component, it is characterized in that: the two ends at this precast body add electric current, by the self-resistance generation heat of precast body.
4, the technology of the long-pending preparation of electric heating process orienting infiltration according to claim 1 charcoal/charcoal component, it is characterized in that: the flow velocity that feeds the gas mixture of Sweet natural gas and nitrogen is 35l/min.
5, the technology of the long-pending preparation of electric heating process orienting infiltration according to claim 1 charcoal/charcoal component is characterized in that: vacuumize to check that the speed that should guarantee to leak gas is less than 0.13Pa/min in the step of whether leaking gas at this.
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| CN101691684B (en) * | 2009-09-23 | 2011-02-09 | 北京航空航天大学 | Preparation and carbonization method of needle-punched pre-oxidative fiber prefabricated part |
| CN101798078B (en) * | 2010-04-22 | 2011-11-09 | 航天材料及工艺研究所 | Quick carbon deposition method of carbon/carbon material member |
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| CN110514005A (en) * | 2019-07-09 | 2019-11-29 | 绵阳宸和电工科技有限公司 | A kind of cvd furnace of Hybrid Heating |
| AU2020360751A1 (en) * | 2019-10-01 | 2022-03-03 | Haldor Topsøe A/S | Cyanide on demand |
| CN112457038A (en) * | 2020-11-13 | 2021-03-09 | 甘肃新西北碳素科技有限公司 | Preparation method of carbon/carbon composite material thin-wall cylinder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101617491B1 (en) * | 2009-12-02 | 2016-05-02 | 비코 인스트루먼츠 인코포레이티드 | Method for improving performance of a substrate carrier and a substrate carrier |
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Assignee: Jiangsu Tianniao High Technology Co., Ltd. Assignor: Beihang University Contract record no.: 2011990000461 Denomination of invention: Process for preparing charcoal/charcoal component by electrothermy orienting infiltration Granted publication date: 20091007 License type: Exclusive License Open date: 20080409 Record date: 20110615 |