CN101671191B - Method for using full preoxidized fiber preform to prepare high-performance carbon-based composite material - Google Patents
Method for using full preoxidized fiber preform to prepare high-performance carbon-based composite material Download PDFInfo
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- CN101671191B CN101671191B CN2009100939517A CN200910093951A CN101671191B CN 101671191 B CN101671191 B CN 101671191B CN 2009100939517 A CN2009100939517 A CN 2009100939517A CN 200910093951 A CN200910093951 A CN 200910093951A CN 101671191 B CN101671191 B CN 101671191B
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Abstract
A method for using full preoxidized fiber to prepare a high-performance carbon-based composite material through rapid directional infiltration includes seven steps: 1. putting the carbonized preoxidized fiber preform in a rapid infiltration furnace and filling graphite gaskets of the same thickness among all discs; 2. vacuumizing the furnace body to minus 0.1Mpa, introducing highly pure nitrogen, freely heating to 1, 000 DEG C and then heating to 1, 800 DEG C according to 100-200 DEG C/h temperature program; 3. freely cooling to set temperature under the protection of nitrogen; 4. stopping introducing nitrogen, vacuumizing the rapid directional infiltration furnace to minus 0.1Mpa and electrically heating a graphite sleeve to conduct constant temperature control on the furnace body; 5. introducing carbon source gas and diluent gas from the furnace bottom mixing carbon source gas and diluent gas according to certain volume rate, extracting the gas from the furnace top and regulating the flow rate of gas according to the total weight of the preforms in the furnace; 6. gradually advancing the infiltration process of the preforms from the inside of the preforms to the outside and obtaining the high-performance carbon-based composite material with the density reaching 1.70-1.80g/cm<3> after 120-200h of one-time infiltration; and 7. vacuumizing the furnace body and cooling freely to room temperature, wherein in the step 5, the pressure in the furnace is subject to certain requirement.
Description
(1) technical field
The present invention relates to a kind of method of full preoxidized fiber preform to prepare high-performance based composite material of carbon, belong to the quick preparing technical field of based composite material of carbon.
(2) background technology
At present, the main raw material of precast body of preparation based composite material of carbon is charcoal fiber and preparatory oxygen silk.Britain Dunlop company adopts preparatory oxygen silk acupuncture mat laminated forming technology preparation based composite material of carbon precast body, and after amassing through the isothermal chemical vapor infiltration, the density of based composite material of carbon reaches 1.75～1.89g/cm
3, the mechanical property of material is on the low side, but friction and wear behavior is good.France Messier-Bugatti adopts acupuncture polyacrylonitrile (PAN), and the Novoltex fabric or the whole felt precast body of the needle-punched carbon fiber forming technique of oxygen silk prepare the based composite material of carbon precast body in advance; After process isothermal chemical vapor infiltration was long-pending, density reached 1.68～1.84g/cm
3, to compare with the based composite material of carbon that Dunlop company prepares, material mechanical performance is suitable, but frictional coefficient is on the low side, and wear rate is higher.514 factories of main office of Aviation Industry of China group adopt needle-punched carbon fiber to prepare the based composite material of carbon precast body; Use the volume(tric)fraction of charcoal fiber to be higher than abroad; With the propylene is the long-pending preparation of carbon-source gas isothermal chemical vapor infiltration based composite material of carbon, and density reaches 1.70～1.80g/cm
3And the materials overseas performance, mechanical property is higher, but friction and wear behavior deviation a little satisfies the requirement of aerospace with based composite material of carbon basically.
The oxygen fiber preform is compared with the charcoal fiber preform in advance; The long-pending fractional precast body (for example volume(tric)fraction is 23%) of low preparatory oxygen filament can obtain than the based composite material of carbon of higher charcoal fiber volume fraction precast body (for example 35%) preparation more excellent friction and wear behavior is arranged after long-pending through chemical vapor infiltration; Be fit to make space shuttle more and use brake material, obtain the favor of the many based composite material of carbon production units in the whole world.Along with in recent years, the increasing that country drops on the charcoal fiber research, but the present domestic processability charcoal fiber suitable with the T300 performance can the more stable preparatory oxygen silks of processability.The oxygen silk prepares when precast body can effectively prevent the acupuncture of Z phase and fracture of wire occurs in advance, and the precast body of preparation is more smooth, and performance is more stable.Because the precast body of oxygen silk preparation oozes the long-pending carbonization that needs before in gas phase in advance; The performance of the preparatory oxygen silk after the carbonization is different with the charcoal fiber; To oozing long-pending technology new requirement has been proposed; The present invention is directed to preparatory oxygen fiber preform special performances, proposed a kind ofly to ooze the long-pending method for preparing high-performance carbon-based composite material by the preparatory oxygen fiber preform slewing after the carbonization.Cheap preparatory oxygen fiber preform cost and fast preparation technology will reduce the cost of high-performance carbon-based composite material significantly.
(3) summary of the invention
1, purpose: the method that the purpose of this invention is to provide a kind of full preoxidized fiber preform to prepare high-performance based composite material of carbon; It is broken through domestic based composite material of carbon and prepares the main restriction of using charcoal fiber production precast body in the process; A kind of long-pending quick preparing technique process of chemical vapor infiltration that preparatory oxygen silk strengthens high-performance carbon-based composite material that is fit to is provided, and slewing is oozed and is long-pendingly prepared density and reach 1.70～1.80g/cm in 200 hours
3High-performance carbon-based composite material, preparation cycle is short, and the precast body preparation cost is low, has reduced the high-performance carbon-based composite material preparation cost significantly.
2, technical scheme: it is as shown in Figure 1 that the method for a kind of full preoxidized fiber preform to prepare high-performance based composite material of carbon of the present invention, its slewing are oozed long-pending stove, and implementation process mainly comprises the following steps:
Step 1: the preparatory oxygen fiber preform after the carbonization is put into slewing and is oozed long-pending stove, and each coils the Graphite pad that is encased inside uniform thickness between the preparatory oxygen fiber preform;
Step 2: body of heater is evacuated to-0.1MPa, feeds high pure nitrogen, and gas feeds from furnace bottom, and furnace roof flows out, and freely is warming up to 1000 ℃, then 100～200 ℃/h temperature programming to 1800 ℃;
Step 3: under nitrogen protection, freely cool to design temperature;
Step 4: stop to feed nitrogen, slewing is oozed long-pending furnace body and is evacuated to-0.1MPa, and electrically heated graphite sleeve carries out thermostatically controlled to body of heater;
Step 5: feed carbon-source gas and diluents, gas is mixed with certain volume ratio, and gas feeds from furnace bottom, and furnace roof is extracted out, and its flow is according to precast body gross weight adjustment in the stove of packing into; The pressure that this slewing is oozed in the long-pending stove is 2kPa～10kPa;
Step 6: the long-pending process of oozing of precast body advances to outside surface from precast body inside gradually, disposablely oozes long-pendingly through 120～200 hours, can make high-performance carbon-based composite material, and density reaches 1.70g/cm
3～1.80g/cm
3
Step 7: body of heater vacuumizes and freely is cooled to room temperature.
Wherein, the preparatory oxygen filament integration number of the precast body of based composite material of carbon described in the step 1 is 22%～27%;
Wherein, the Graphite pad of the uniform thickness described in the step 1, its thickness are 1.5mm～5mm, and this Graphite pad is placed in the precast body outer rim, equidistant placement;
Wherein, the preparatory oxygen fiber preform described in the step 1 after the carbonization is put into slewing and is oozed long-pending stove, once can lay preparatory oxygen fiber preform 30 dishes～50 dishes;
Wherein, feed high pure nitrogen described in the step 2, the purity of its nitrogen is greater than 99.9%; The flow of nitrogen is 100～200L/h;
Wherein, freely cool to design temperature described in the step 3, cool to preparatory oxygen fiber preform peripheral temperature and reach 1080 ℃～1130 ℃, oxygen fiber preform core temperature reaches 1020 ℃～1080 ℃ in advance;
Wherein, the carbon-source gas described in the step 5 is Sweet natural gas and propane gas mixture, and diluents is a hydrogen; The volume ratio of Sweet natural gas and propane is 6～9: 1; The volume ratio of hydrogen and propane is 1～5: 1;
Wherein, flow described in the step 5 is meant that according to precast body gross weight adjustment in the stove of packing into control per hour required carbon-source gas Sweet natural gas of per kilogram precast body and propane gross weight are 50g～100g;
Wherein, body of heater vacuumizes described in the step 7, and its vacuum tightness is-0.1MPa.
3, advantage and effect: the present invention compared with prior art, its advantage and effect are:
(1) the present invention adopts the preoxidized fiber preform to prepare high-performance carbon based composites, and oxygen silk market value is lower than the charcoal fiber in advance at present, thereby selects for use preparatory oxygen silk to reduce the preparation cost of high-performance carbon-based composite material.
(2) the precast body surfacing of adopting preparatory oxygen silk to prepare, Z is to good heat conductivity, and friction and wear behavior is good, is particularly suitable for doing aviation and uses friction element.
(3) the employing Sweet natural gas of innovation and propane gas mixture are as carbon-source gas, and hydrogen has improved the utilization ratio of precursor gas as diluents, has further reduced the preparation cost of material.
(4) adopt the present invention's technology, can prepare density in 200 hours and reach 1.70～1.80g/cm
3High-performance carbon-based composite material, pyrolytic carbon is mainly rough layer.Compare with traditional isothermal process, shortened preparation cycle.
(4) description of drawings
Long-pending furnace structure synoptic diagram is oozed in the slewing of Fig. 1 high-performance carbon-based composite material
The scheme of installation of Fig. 2 pad
Description of reference numerals
The 1-air outlet; 2-oozes long-pending furnace wall; 3-heating graphite sleeve;
4-graphite cover plate; The 5-Graphite pad; The preparatory oxygen fiber preform of 6-;
7-graphite guiding device; The 8-through hole; 9-graphite plectane;
10-graphite plectane with holes; The 11-pad; The 12-graphite cylinder;
The 13-inlet mouth.
(5) embodiment
The method of a kind of full preoxidized fiber preform to prepare high-performance based composite material of carbon of the present invention, this method specific embodiment is following:
Embodiment 1
The method of a kind of full preoxidized fiber preform to prepare high-performance based composite material of carbon of the present invention, these method concrete steps are following:
The long-pending equipment of its chemical vapor infiltration is as shown in Figure 1, and method of the present invention is oozed in the pneumatosis flow control device in this high-performance carbon-based composite material slewing and carried out.
Step 1: the preparatory oxygen fiber preform 6 after the carbonization is put into slewing and is oozed long-pending stove, and external diameter is 420mm, and internal diameter is 250mm; Thickness is 24mm; Initial oxygen filament integration in advance is several 22%, steadily is placed on the graphite plectane 9, fills up with Graphite pad 5 between the every precast body and opens; Once pack into 40 of graphite precast bodies, and cover graphite cover plate 4.The placement location of Graphite pad 5 is as shown in Figure 2, and the thickness of Graphite pad 5 is 1.5mm.
Step 2: body of heater is evacuated to-0.1MPa, feeds purity greater than 99.9% high pure nitrogen, and gas feeds from furnace bottom, and furnace roof flows out, and the flow of nitrogen is 100L/h, freely is warming up to 1000 ℃, then 100 ℃/h temperature programming to 1800 ℃;
Step 3: under nitrogen protection, freely cool to preparatory oxygen fiber preform peripheral temperature and reach 1080 ℃, oxygen fiber preform core temperature reaches 1030 ℃ in advance;
Step 4: stop to feed nitrogen, slewing is oozed long-pending furnace body and is evacuated to-0.1MPa, and electrically heated graphite sleeve carries out thermostatically controlled to body of heater;
Step 5: the mixed gas and the diluents hydrogen of carbon-source gas Sweet natural gas and propane are oozed long-pending stove through inlet mouth 13 feedings; The total flux of carbon-source gas is looked the total flux of precast body and is decided; The per kilogram precast body per hour feeds carbon-source gas 80g; The volume ratio of Sweet natural gas and propane is 8/1, and the volume ratio of propane and diluents hydrogen is 1/1, and the furnace pressure that long-pending stove is oozed in control is 5kPa.
Step 6: oozed long-pending 160 hours, the density of based composite material of carbon just can reach 1.72～1.76g/cm
3
Step 7: body of heater vacuumizes and freely is cooled to room temperature.Its vacuum tightness is-0.1MPa.
Embodiment 2
The method of a kind of full preoxidized fiber preform to prepare high-performance based composite material of carbon of the present invention, these method concrete steps are following:
The long-pending equipment of its chemical vapor infiltration is as shown in Figure 1, and method of the present invention is oozed in the pneumatosis flow control device in this high-performance carbon-based composite material slewing and carried out.
Step 1: the preparatory oxygen fiber preform 6 after the carbonization is put into slewing and is oozed long-pending stove, and external diameter is 450mm, and internal diameter is 270mm; Thickness is 22mm; Initial oxygen filament integration in advance is several 25%, steadily is placed on the graphite plectane 9, fills up with Graphite pad 5 between the every precast body and opens; Once pack into 30 of graphite precast bodies, and cover graphite cover plate 4.The placement location of Graphite pad 5 is as shown in Figure 2, and the thickness of Graphite pad 5 is 1.5mm.
Step 2: body of heater is evacuated to-0.1MPa, feeds purity greater than 99.9% high pure nitrogen, and gas feeds from furnace bottom, and furnace roof flows out, and the flow of nitrogen is 100L/h, freely is warming up to 1000 ℃, then 100 ℃/h temperature programming to 1800 ℃;
Step 3: under nitrogen protection, freely cool to preparatory oxygen fiber preform peripheral temperature and reach 1070 ℃, oxygen fiber preform core temperature reaches 1020 ℃ in advance;
Step 4: stop to feed nitrogen, slewing is oozed long-pending furnace body and is evacuated to-0.1MPa, and electrically heated graphite sleeve carries out thermostatically controlled to body of heater;
Step 5: the mixed gas and the diluents hydrogen of carbon-source gas Sweet natural gas and propane are oozed long-pending stove through inlet mouth 13 feedings; The total flux of carbon-source gas is looked the total flux of precast body and is decided; The per kilogram precast body per hour feeds carbon-source gas 50g; The volume ratio of Sweet natural gas and propane is 8/1, and the volume ratio of propane and diluents hydrogen is 1/1, and the furnace pressure that long-pending stove is oozed in control is 5kPa.
Step 6: oozed long-pending 190 hours, the density of based composite material of carbon just can reach 1.73g/cm
3～1.80g/cm
3；
Step 7: body of heater vacuumizes and freely is cooled to room temperature.Its vacuum tightness is-0.1MPa.
Claims (7)
1. the method for a full preoxidized fiber preform to prepare high-performance based composite material of carbon, it is characterized in that: these method concrete steps are following:
Step 1: the preparatory oxygen fiber preform after the carbonization is put into slewing ooze long-pending stove, each coils the Graphite pad that is encased inside uniform thickness between the preparatory oxygen fiber preform;
Step 2: body of heater is evacuated to-0.1MPa, feeds high pure nitrogen, and gas feeds from furnace bottom, and furnace roof flows out, and freely is warming up to 1000 ℃, then by 100～200 ℃/h temperature programming to 1800 ℃;
Step 3: under nitrogen protection, freely cool to design temperature; Design temperature is that preparatory oxygen fiber preform peripheral temperature reaches 1080 ℃～1130 ℃, and the preheating unit core temperature reaches 1020 ℃～1080 ℃;
Step 4: stop to feed nitrogen, slewing is oozed long-pending furnace body and is evacuated to-0.1MPa, and electrically heated graphite sleeve carries out thermostatically controlled to body of heater;
Step 5: feed carbon-source gas and diluents, gas is mixed with certain volume ratio, and gas feeds from furnace bottom, and furnace roof is extracted out, and its flow is according to precast body gross weight adjustment in the stove of packing into, and furnace pressure has requirement; The said carbon-source gas of selecting for use is Sweet natural gas and propane gas mixture, and diluents is a hydrogen; The volume ratio of Sweet natural gas and propane is 6～9: 1; The volume ratio of hydrogen and propane is 1～5: 1; Said flow is meant that according to precast body gross weight adjustment in the stove of packing into control per hour required carbon-source gas Sweet natural gas of per kilogram precast body and propane gross weight are 50g～100g; The pressure that said slewing is oozed in the long-pending stove is 2kPa～10kPa;
Step 6: the long-pending process of oozing of precast body advances to outside surface from precast body inside gradually, disposablely oozes long-pendingly through 120～200 hours, promptly makes high-performance carbon-based composite material, and density reaches 1.70g/cm
3～1.80g/cm
3
Step 7: body of heater vacuumizes and freely is cooled to room temperature.
2. the method for a kind of full preoxidized fiber preform to prepare high-performance based composite material of carbon according to claim 1 is characterized in that: the preparatory oxygen filament integration number of precast body is 22%～27% in the step 1.
3. the method for a kind of full preoxidized fiber preform to prepare high-performance based composite material of carbon according to claim 1 is characterized in that: the thickness of the Graphite pad described in the step 1 is 1.5mm～5mm, and pad is placed in the precast body outer rim, equidistant placement.
4. the method for a kind of full preoxidized fiber preform to prepare high-performance based composite material of carbon according to claim 1 is characterized in that: lay preparatory oxygen fiber preform 30 dishes～50 dishes in the step 1.
5. the method for a kind of full preoxidized fiber preform to prepare high-performance based composite material of carbon according to claim 1 is characterized in that: the purity of nitrogen described in the step 2 is greater than 99.9%.
6. the method for a kind of full preoxidized fiber preform to prepare high-performance based composite material of carbon according to claim 1 is characterized in that: the flow of nitrogen described in the step 2 is 100～200L/h.
7. the method for a kind of full preoxidized fiber preform to prepare high-performance based composite material of carbon according to claim 1 is characterized in that: body of heater vacuumizes described in the step 7, and its vacuum tightness is-0.1MPa.
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| CN102020482B (en) * | 2010-11-13 | 2013-10-16 | 西安超码科技有限公司 | Large resistive double-vacuum gas-phase carbon deposition device |
| CN102433543B (en) * | 2011-12-20 | 2013-08-14 | 西安超码科技有限公司 | Multi-deposition-chamber CVI (chemical vapor infiltration) device for compacting carbon/carbon crucible and method using same |
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| US4950558A (en) * | 1987-10-01 | 1990-08-21 | Gte Laboratories Incorporated | Oxidation resistant high temperature thermal cycling resistant coatings on silicon-based substrates and process for the production thereof |
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