CN102010219B - Method for preparing carbon/carbon composite material by liquid precursor atomization - Google Patents
Method for preparing carbon/carbon composite material by liquid precursor atomization Download PDFInfo
- Publication number
- CN102010219B CN102010219B CN2010105168833A CN201010516883A CN102010219B CN 102010219 B CN102010219 B CN 102010219B CN 2010105168833 A CN2010105168833 A CN 2010105168833A CN 201010516883 A CN201010516883 A CN 201010516883A CN 102010219 B CN102010219 B CN 102010219B
- Authority
- CN
- China
- Prior art keywords
- carbon
- graphite heater
- precast body
- compound material
- reactor drum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Abstract
The invention discloses a method for preparing a carbon/carbon composite material by liquid precursor atomization. The method comprises: a multiple-point pressure spraying device is adopted to inject precursors into a reactor and a precast body in a liquefaction spraying way, and liquid phase-atomization-gasification rapid deposition is carried out, thus obtaining the carbon/carbon composite material with the density of 1.6-1.8g/cm<3>.The invention has the advantages that the liquid precursor boiling gasification link is omitted, the energy consumption is reduced, and the controllability of precursor concentration and feeding is realized, the control and regulation of liquid hydrocarbon precursor amount are easier, the utilization factor of liquid hydrocarbon is greatly improved, the effect is obvious in trial-production, and the carbon/carbon composite material with the density reaching up to 1.8g/cm<3> is prepared in 8 hours successfully.
Description
Technical field:
The invention belongs to field of compound material, relate to a kind of fast preparation method of matrix material, especially a kind of is the method that carbon source prepares carbon/carbon compound material with the liquid precursor aerosol.
Background technology:
Carbon/carbon compound material (C/C; Carbon/carbon composites) leading edge of a wing, nose cone, the jet pipe of thrust chamber, the larynx lining of space shuttle have been widely used in; And the retarding disc of aircraft, it is irreplaceable in the effect of aerospace field as high-temperature structural material and building blocks of function.Prepare at present the up-to-date method of carbon/carbon and is chemical liquid phase gasify osmosis (Chemical liquid-vaporized infiltration, CLVI, or be called as Film boiling CVI; FBCVI), with carbon/carbon compound material traditional preparation method chemical vapor infiltration (Chemical vapor infiltration, CVI) and liquid phase (resin; Pitch) the dipping carborization is compared; Densification rate is the highest, has shortened the time of preparation carbon/carbon compound material greatly, has reduced preparation cost.
Existing CLVI method all is that precast body is wrapped in around the heating element, and immerses in the liquid precursor (like hexanaphthene, kerosene etc.) with heating element.Through the mode of induction heating mode or resistive heating, liquid precursor produces bigger thermal gradient from inside to outside.Temperature reaches more than 800 ℃ when the precast body inboard, and the liquid precursor in the immersion precast body hole is generating gasification, scission reaction successively, generates RESEARCH OF PYROCARBON at carbon fiber surface.With the reaction times prolongation, pass from the precast body inboard gradually laterally in the densification forward position, accomplishes the densification of precast body, blowing out in the middle of process need not.The fast densified reason of CLVI can be summed up as: (1) precursor (carbon source) is to the rapid osmotic and the diffusion in densification forward position; (2) the inner big thermal gradient of precast body.
But also there is certain defective in the CLVI method of announcing at present, mainly shows:
(1) because the complicacy of process and liquid severity of driving body boiling-gasification; Make in the deposition process; The concentration of reactant gases is difficult to control and calculates; So that particularity and the exactness of result of study are not high, and the repeatability of the feasible product that makes and the suitability for industrialized production of technology all are restricted.
(2) because the complicacy of the boiling-gasification of liquid precursor; Make that the gas concentration in the sediment chamber is inhomogeneous; The carbon/carbon compound material nacrostructure that also just causes making receives the limitation of heating element shape; Mostly be the shape of comparison rule, just be difficult to reach the requirement of use for odd-shaped carbon/carbon compound material member.
(3) in the CLVI densified carbon/carbon composite material process, precast body and heating element are immersed in the liquid precursor all the time.This process receives complicated chemical reaction, thermal conduction study, thermodynamics of reactions, hydromeehanics, boiling heat transfer and influences jointly; Therefore carbon/carbon composite wood the micro-structure and property that makes and the relation between the apparent processing parameter are difficult to give theoretically explain and calculate accurately, and realization and the control to processing parameter is also very difficult in the actually operating.
(4) consider from the angle of energy consumption and efficient; Make liquid precursor in precast body, form successive gaseous film (being film boiling) and scission reaction generation deposit carbon; The huge heating power that needs has sufficiently high temperature and long time to guarantee the precast body inboard, has so both caused a large amount of wastes of electric energy and liquid precursor.
Therefore be necessary to the CLVI further improvements in methods.
Summary of the invention:
To the defective or the deficiency that exist in the above-mentioned existing CLVI method, the object of the present invention is to provide the liquid precursor atomizing to prepare the method for carbon/carbon compound material.This method can reach: atomization quantity can be controlled through some valves owing to used atomisation unit in (1), thereby realizes the accurate control to reactant concn.(2) nacrostructure of carbon/carbon compound material of preparation is various, and can make what satisfy performance and request for utilization mainly is the carbon/carbon compound material of polymorphic structure.(3) position of atomisation unit can be arranged flexibly, and the liquid precursor of atomizing is evenly distributed in the sediment chamber, thereby by even heating and gasification, obtains the uniform carbon/carbon compound material of microtexture.(4) effectively prevent a small amount of condensation of liquid precursor in the preparation process, realized further improving the utilization ratio of liquid low molecular hydrocarbon; (5) type of heating of this method not only can be a resistive heating but also can be induction heating.
Technical solution of the present invention is following:
A kind of liquid precursor atomizing prepares the method for carbon/carbon compound material; Said method is to adopt multipoint mode press atomization device that presoma is sprayed in reactor drum and the precast body with the liquefaction spray pattern, the liquid phase presoma pass through atomizing-gasification-Pintsch process and fast deposition to obtain density be 1.6-1.8g/cm
3Carbon/carbon compound material.
Said presoma is hexanaphthene or kerosene.
Said precast body is made up of carbon fiber porous structure.
A kind of liquid precursor atomizing prepares the method for carbon/carbon compound material, comprises the steps:
(1) preparation porous preform: the carbon fiber knit system that will have porous carbon felt, carbon cloth, 2D carbon fiber knit body or 3D becomes the precast body of desired shape and size;
(2) preparation graphite heater and annex thereof: according to the size of porous preform, common graphite is processed into cylindrical graphite heater or rectangular parallelepiped, confirms the mode of precast body placement and the quantity of placement according to the position of space in the reactor drum and graphite heater;
(3) graphite heater and porous preform are put into reactor drum successively, guarantee that porous preform one side closely contacts with the heating element hot face, form the high-temperature zone, guarantee that heating fully;
(4) condenser cover with chemical liquid phase vapor deposition device also seals on reactor drum; Start oil-sealed rotary pump; The reactor drum air is evacuated to below the 1kPa, stops vacuum pump, in reactor drum, fill N2 to normal atmosphere of shielding gas through protection gas inlet then; Open the air outlet, and guarantee that the flow of shielding gas is 10～40 liters/hour; Start cooling system;
(5) start heating power supply, through graphite heater heating porous preform; Heat-processed makes the temperature of its high-temperature zone rise to 900 ℃ through the temperature of the inboard high-temperature zone of thermocouple measurement porous preform;
(6) in reaction chamber, spray mist attitude presoma through liquid precursor make up system and atomisation unit, through the concentration of the gas inside the atomisation unit controlling reactor;
(7) keep precast body high-temperature zone temperature at 900 ℃-1350 ℃, spraying continuously, deposition reaction 2-8 hour, and according to the kerosene in adjustment in time of precursor concentration in the reaction chamber and the additional atomisation unit;
(8) stop atomisation unit successively, heating power supply, be cooled to room temperature after, stop shielding gas N again
2And condenser cooling water;
(9) open condensing surface, take out the graphite heater precast body good in the reactor drum with deposition;
(10) graphite heater, deposition precast body are well cut along contact surface, promptly obtain density 1.6-1.8g/cm
3Carbon/carbon compound material, and carbon/carbon compound material further detected, processes, obtain product.
It is wherein a kind of that described liquid low molecular hydrocarbon is selected from kerosene, gasoline, diesel oil, hexanaphthene.
Described shielding gas is selected from nitrogen or argon gas.
Described porous preform be shaped as different shapes such as annular, disc, bulk.
Described heating power supply is resistive heating or induction heating.
Described atomisation unit can be multiple spot pressure type or centrifugal multi-stage type or compressed air type or rotary.
A kind of liquid precursor atomizing prepares the method for carbon/carbon compound material:
(1) prepare precast body 101, will have porous carbon felt, carbon cloth, and 2D or 3D carbon fiber knit system become certain size and shape;
(2) prepare graphite heater 102 and annex 103 thereof; According to precast body and the size of keeping for mist attitude precursor heating space; Confirm the size and the size of graphite heater; The material of graphite heater adopts commercially available common graphite, simultaneously according to reaction chamber space size prepare a certain size with the shape lagging material (103, the protection body of heater;
(3) lagging material 103, graphite heater (102) and precast body 101 are put into reactor drum in order, guarantee that precast body one side closely contacts with the heating element hot face, form the high-temperature zone, guarantee that heating fully;
(4) be placed on the reactor drum 105 condensing surface 104 and sealing; Start oil-sealed rotary pump 106, the reactor drum air is evacuated to negative pressure, stop vacuum pump; In reactor drum 105, fill protection gas to one normal atmosphere through protection gas inlet 107 then; Open air outlet 108, and the flow that guarantees protection gas be the 10-40 liter/hour, start condenser cooling water;
(5) start heating power supply 109, through ruhmkorff coil 110 heating graphite heaters 102, heat-processed makes the temperature of its high-temperature zone rise to 900 ℃ through the temperature of the inboard high-temperature zone of thermopair 111 measurement porous preforms;
(6) in reactor drum 110, spray mist attitude presoma through liquid precursor make up system 111 and atomisation unit 112, through the concentration of the gas inside the atomisation unit controlling reactor;
(7) keep precast body high-temperature zone temperature at 900 ℃-1350 ℃, spraying continuously, deposition reaction 2-8 hour, and according to timely adjustment of precursor concentration in the reaction chamber and additional kerosene;
(8) stop atomisation unit 112 successively earlier, stop heating power supply 109 again, be cooled to room temperature after, stop shielding gas N
2(107) and condenser cooling water 113;
(9) furnace cooling is opened condensing surface 104 to room temperature, takes out graphite heater 102 and fine and close carbon/carbon compound material 101 successively;
(10) graphite heater 102 and carbon/carbon compound material 101 are cut along contact surface, and carbon/carbon compound material 101 is further detected, processes, obtain the finished product.
A kind of liquid precursor atomizing prepares the method for carbon/carbon compound material,
(1) prepares porous preform, the 2D thomel is cut to an external diameter Φ 150mm, internal diameter Φ 100mm, the hollow circular cylinder of high 100mm;
(2) prepare graphite heater and annex thereof, graphite heater is processed as Φ 100mm diameter, thickness is 110mm, prepares a certain size and shape lagging material simultaneously, the protection body of heater;
(3) lagging material, graphite heater, porous preform are put into reactor drum in order, make next two objects, guarantee that precast body one side closely contacts with the heating element hot face, guarantee that heating fully in the coaxial placement of reaction chamber;
(4) with condenser cover also sealing on reactor drum, start oil-sealed rotary pump, reactor drum air pressure is evacuated to below the 1kPa, stop vacuum pump, in reactor drum, fill N through protection gas inlet then
2To a normal atmosphere, open the air outlet, and guarantee N
2Influx be 20 liters/hour (minimum is not less than 10 liters/hour, is 40 liters/hour to the maximum), start condenser cooling water;
(5) start induction heating power, the heating graphite heater, heat-processed makes the temperature of its high-temperature zone rise to 900 ℃ through the temperature of the inboard high-temperature zone of thermocouple measurement porous preform;
(6) in reactor drum, spray mist attitude presoma through liquid precursor make up system and atomisation unit, through the concentration of the gas inside the multipoint mode press atomization device controlling reactor;
(7) keep precast body high-temperature zone temperature at 900 ℃-1350 ℃, spraying continuously, deposition reaction 2-8 hour, and according to timely adjustment of precursor concentration in the reaction chamber and additional kerosene;
(8) stop atomisation unit successively, and heating power supply, be cooled to room temperature after, stop shielding gas N again
2And condenser cooling water;
(9) furnace cooling is opened condensing surface to room temperature, takes out graphite heater and fine and close carbon/carbon compound material successively;
(10) graphite heater and carbon/carbon compound material are cut along contact surface, and carbon/carbon compound material is further detected, processes, obtain the finished product, the mean density of the annular carbon/carbon material of the 2D thomel base of acquisition is 1.8g/cm
3
The liquid precursor atomizing prepares the method for carbon/carbon compound material, is characterized in that liquid precursor does not directly contact with precast body.Liquid precursor is ejected into reaction chamber uniformly with the atomizing attitude; Heating element heating precast body in the reaction chamber; The precursor of radiating heat atomizing simultaneously and can realize gasification; And form big thermal gradient at the thickness direction of precast body, for the gaseous carbon source scission reaction and form RESEARCH OF PYROCARBON enough temperature are provided.
In suitability for industrialized production, to use method of the present invention and prepare carbon/carbon compound material, its meliority is mainly reflected in:
(1) characteristics of the present invention's essence are that the precast body of carbon fiber knit body or carbon felt, carbon cloth or its combination was processed density in 2-8 hour reach 1.6-1.8g/cm fast
3Carbon/carbon compound material;
(2) there is big thermal gradient in the precast body of the present invention, guaranteed higher sedimentation rate, only need once just can accomplish deposition.
(3) great advantage of the existing CLVI technology of the present invention is: can be through reasonable arrangement and the control to atomisation unit; Be easy to the controllability of realization response gas concentration, pressure and other parameters, also can carry out the feed of intermittent type (pulsed) as required; Increase the reactant concn gradient;
(4) the liquid precursor of the present invention heats with the state of atomizing, has simplified gasification, has reduced the gasification energy needed, improves the precursor utilization ratio, and improves the liquid precursor utilization ratio;
(5) type of heating of the present invention is free, and resistance and induction heating can.
(6) graphite heater can reuse, through changing the preparation that the big I of heating element realizes the carbon/carbon compound material of different size size and shape.
(7) heating elements can heat simultaneously and difform carbon/carbon compound material, can save current consumption greatly.
Description of drawings:
Fig. 1 is that the present invention adopts the induction heating single hollow circuit cylinder carbon/carbon compound material schematic representation of apparatus of preparation fast;
Fig. 2 is that the present invention adopts the resistive heating synoptic diagram of four block carbon/carbon compound materials of preparation fast;
Wherein: 101 be the hollow circuit cylinder precast body, 102 for the cylinder graphite heater, 103 for lagging material, 104 for condensing surface, 105 for reaction chamber, 106 for oil-sealed rotary pump, 107 for protection gas inlet, 108 for reaction gas outlet, 109 for induction heating power, 110 for ruhmkorff coil, 111 for thermopair, 112 for multipoint mode press atomization device, 113 for cooling water outlet and inlet, 114 for the liquid precursor deposit with replenish inlet.
201 first block precast bodies, 203 second block precast bodies, 204 the 3rd block precast bodies, 206 be the 4th block precast body, 202 be the first blocky graphite heating element, 205 be the second blocky graphite heating element, 207 first lagging materials, 208 be second lagging material, 209 for condensing surface, 210 for reaction chamber, 211 for oil-sealed rotary pump, 212 for protection gas inlet, 213 for reaction gas outlet, 214 and 215 is the resistive heating power supply,, 216 be thermal insulation layer, 217 for thermopair, 218 for centrifugal multi-stage type spraying plant, 219 for the liquid precursor deposit with replenish and enter the mouth.
Embodiment:
Below in conjunction with accompanying drawing the present invention is done and to describe in further detail:
Referring to Fig. 1 and 2; The present invention has adopted a kind of and the diverse mentality of designing of forefathers' technology; Liquid precursor is ejected into the sediment chamber uniformly with the atomizing attitude, heating element in sediment chamber heating precast body, the precursor of radiating heat atomizing simultaneously and can realize gasification.
Below in conjunction with accompanying drawing 1, the detailed process for preparing single carbon/carbon compound material for the present invention is described below:
(1) prepare precast body 101, will have porous carbon felt, carbon cloth, and 2D or 3D carbon fiber knit system become certain size and shape;
(2) prepare graphite heater 102 and annex 103 thereof; According to precast body and the size of keeping for mist attitude precursor heating space; Confirm the size and the size of graphite heater; The material of graphite heater adopts commercially available common graphite, simultaneously according to reaction chamber space size prepare a certain size with the shape lagging material (103, the protection body of heater;
(3) lagging material 103, graphite heater 102 and precast body 101 are put into reactor drum in order, guarantee that precast body one side closely contacts with the heating element hot face, form the high-temperature zone, guarantee that heating fully;
(4) be placed on the reactor drum 105 condensing surface 104 and sealing; Start oil-sealed rotary pump 106, the reactor drum air is evacuated to negative pressure, stop vacuum pump; In reactor drum 105, fill protection gas to one normal atmosphere through protection gas inlet 107 then; Open air outlet 108, and the flow that guarantees protection gas be the 10-40 liter/hour, start condenser cooling water;
(5) start heating power supply 109, through ruhmkorff coil 110 heating graphite heaters 102, heat-processed makes the temperature of its high-temperature zone rise to 900 ℃ through the temperature of the inboard high-temperature zone of thermopair 111 measurement porous preforms;
(6) in reactor drum 110, spray mist attitude presoma through liquid precursor make up system 111 and atomisation unit 112, through the concentration of the gas inside the atomisation unit controlling reactor;
(7) keep precast body high-temperature zone temperature at 900 ℃-1350 ℃, spraying continuously, deposition reaction 2-8 hour, and according to timely adjustment of precursor concentration in the reaction chamber and additional kerosene;
(8) stop atomisation unit 112 successively earlier, stop heating power supply 109 again, be cooled to room temperature after, stop shielding gas N
2107 with condenser cooling water 113;
(9) furnace cooling is opened condensing surface 104 to room temperature, takes out graphite heater 102 and fine and close carbon/carbon compound material 101 successively;
(10) graphite heater 102 and carbon/carbon compound material 101 are cut along contact surface, and carbon/carbon compound material 101 is further detected, processes, obtain the finished product.。
In conjunction with accompanying drawing 2, the graphite heater and the porous preform specification that the present invention are prepared simultaneously four block carbon/carbon compound materials are following:
For preparing four block carbon/carbon compound materials (201,203,204 and 206); Adopt the mode of two blocky graphite heating elements (202 and 205) and resistive heating; Carbon/carbon compound material (201 and 203) is placed on the both sides of graphite heater 202; And keep closely contact, carbon/carbon compound material (204 and 206) is placed on the both sides of graphite heater 205, and keeps closely contact; Spraying plant can suitably be adjusted according to actual condition, and other process step is identical with the description of above-mentioned preparation single-piece carbon/carbon compound material.
The contriver provides following embodiment, but the invention is not restricted to these embodiment.
Embodiment 1: according to technical scheme of the present invention, in conjunction with accompanying drawing 1, the carbon felt that adopts the charcoal ink factory, Lanzhou to produce is a precast body, and carbon felt density is 0.1g/cm
3, form by any direction staple fibre.Adopt the concrete steps of a hollow cylinder carbon/carbon compound material of method preparation of the present invention following:
(1) prepares porous preform, the 2D thomel is cut to an external diameter Φ 150mm, internal diameter Φ 100mm, the hollow circular cylinder of high 100mm;
(2) prepare graphite heater and annex thereof, graphite heater is processed as Φ 100mm diameter, thickness is 110mm, prepares a certain size and shape lagging material simultaneously, the protection body of heater;
(3) lagging material, graphite heater, porous preform are put into reactor drum in order, make next two objects, guarantee that precast body one side closely contacts with the heating element hot face, guarantee that heating fully in the coaxial placement of reaction chamber;
(4) with condenser cover also sealing on reactor drum, start oil-sealed rotary pump, reactor drum air pressure is evacuated to below the 1kPa, stop vacuum pump, in reactor drum, fill N through protection gas inlet then
2To a normal atmosphere, open the air outlet, and guarantee N
2Influx be 20 liters/hour (minimum is not less than 10 liters/hour, is 40 liters/hour to the maximum), start condenser cooling water;
(5) start induction heating power, the heating graphite heater, heat-processed makes the temperature of its high-temperature zone rise to 900 ℃ through the temperature of the inboard high-temperature zone of thermocouple measurement porous preform;
(6) in reactor drum, spray mist attitude presoma through liquid precursor make up system and atomisation unit, through the concentration of the gas inside the multipoint mode press atomization device controlling reactor;
(7) keep precast body high-temperature zone temperature at 900 ℃-1350 ℃, spraying continuously, deposition reaction 2-8 hour, and according to timely adjustment of precursor concentration in the reaction chamber and additional kerosene;
(8) stop atomisation unit successively, and heating power supply, be cooled to room temperature after, stop shielding gas N again
2And condenser cooling water;
(9) furnace cooling is opened condensing surface to room temperature, takes out graphite heater and fine and close carbon/carbon compound material successively;
(10) graphite heater and carbon/carbon compound material are cut along contact surface, and carbon/carbon compound material is further detected, processes, obtain the finished product, the mean density of the annular carbon/carbon material of the 2D thomel base of acquisition is 1.8g/cm
3, cylinder outer edge density difference is merely 0.02g/cm
3
Embodiment 2: according to technical scheme of the present invention, in conjunction with accompanying drawing 2, adopting the 2D thomel of PAN-3k is porous preform, and density is 0.5g/cm
3Adopt the concrete steps of four blocky carbon/carbon compound materials of method preparation of the present invention following:
(1) prepares porous preform, the 2D thomel is cut to four 100 * 100 * 20mm
3Cuboid;
(2) prepare graphite heater and annex thereof, graphite heater is processed as two 120 * 100 * 30mm
3Cuboid, simultaneously prepare a certain size and shape lagging material, the protection body of heater according to reaction chamber space size;
(3) lagging material, graphite heater, porous preform are put into reactor drum in order, guarantee that precast body one side closely contacts with the heating element hot face, form the high-temperature zone, guarantee that heating fully;
(4) with condenser cover also sealing on reactor drum, start oil-sealed rotary pump, reactor drum air pressure is evacuated to below the 1kPa, stop vacuum pump, in reactor drum, fill N through protection gas inlet then
2To a normal atmosphere, open the air outlet, and guarantee N
2Influx be 20 liters/hour (minimum is not less than 10 liters/hour, is 40 liters/hour to the maximum), start condenser cooling water;
(5) starting resistance heating power supply, the heating graphite heater, heat-processed makes the temperature of its high-temperature zone rise to 900 ℃ through the temperature of the inboard high-temperature zone of thermocouple measurement porous preform;
(6) in reactor drum, spray mist attitude presoma through liquid precursor make up system and atomisation unit, through the concentration of the gas inside the multipoint mode press atomization device controlling reactor;
(7) keep precast body high-temperature zone temperature at 900 ℃-1350 ℃, spraying continuously, deposition reaction 6 hours, and according to the kerosene in adjustment in time of precursor concentration in the reaction chamber and the additional atomisation unit;
(8) stop atomisation unit successively, heating power supply, be cooled to room temperature after, stop shielding gas N again
2And condenser cooling water;
(9) furnace cooling is opened condensing surface to room temperature, takes out the graphite heater carbon/carbon compound material good with deposition in the reaction chamber successively;
(10) graphite heater, deposition carbon/carbon compound material are well cut along contact surface, and carbon/carbon compound material is further detected, processes, obtain the finished product, the mean density of the rectangle carbon/carbon material of the 2D thomel base of acquisition is 1.7g/cm
3
Above content is to combine concrete preferred implementation to further explain that the present invention did; Can not assert that embodiment of the present invention only limits to this; Those of ordinary skill for technical field under the present invention; Under the prerequisite that does not break away from the present invention's design, can also make some simple deduction or replace, all should be regarded as belonging to the present invention and confirm scope of patent protection by claims of being submitted to.
Claims (7)
1. a liquid precursor atomizes and prepares the method for carbon/carbon compound material; It is characterized in that: said method is to adopt multipoint mode press atomization device that presoma is sprayed in reactor drum and the precast body with the liquefaction spray pattern, the liquid phase presoma pass through atomizing-gasification-Pintsch process and fast deposition to obtain density be 1.6-1.8g/cm
3Carbon/carbon compound material.
2. a kind of according to claim 1 liquid precursor atomizing prepares the method for carbon/carbon compound material, and it is characterized in that: said presoma is hexanaphthene and kerosene.
3. a kind of according to claim 1 liquid precursor atomizing prepares the method for carbon/carbon compound material, and it is characterized in that: said precast body is made up of carbon fiber porous structure.
4. a kind of according to claim 1 liquid precursor atomizing prepares the method for carbon/carbon compound material, it is characterized in that, comprises the steps:
(1) preparation porous preform: the carbon fiber knit system that will have porous carbon felt, carbon cloth, 2D carbon fiber knit body or 3D becomes the precast body of desired shape and size;
(2) preparation graphite heater and annex thereof: according to the size of porous preform, common graphite is processed into cylindrical graphite heater or rectangular parallelepiped, confirms the mode of precast body placement and the quantity of placement according to the position of space in the reactor drum and graphite heater;
(3) graphite heater and porous preform are put into reactor drum successively, guarantee that porous preform one side closely contacts with the heating element hot face, form the high-temperature zone, guarantee that heating fully;
(4) with condenser cover also sealing on reactor drum of chemical liquid phase vapor deposition device, start oil-sealed rotary pump, the reactor drum air is evacuated to below the 1kPa, stop vacuum pump, in reactor drum, fill shielding gas N through protection gas inlet then
2To a normal atmosphere, open the air outlet, and guarantee that the flow of shielding gas is 10 ~ 40 liters/hour; Start cooling system;
(5) start heating power supply, through graphite heater heating porous preform; Heat-processed makes the temperature of its high-temperature zone rise to 900 ℃ through the temperature of the inboard high-temperature zone of thermocouple measurement porous preform;
(6) in reaction chamber, spray mist attitude presoma through liquid precursor make up system and atomisation unit, through the concentration of the gas inside the atomisation unit controlling reactor;
(7) keep precast body high-temperature zone temperature at 900 ℃-1350 ℃, spraying continuously, deposition reaction 2-8 hour, and according to the kerosene in adjustment in time of precursor concentration in the reaction chamber and the additional atomisation unit;
(8) stop atomisation unit successively, heating power supply, be cooled to room temperature after, stop shielding gas N again
2And condenser cooling water;
(9) open condensing surface, take out the graphite heater precast body good in the reactor drum with deposition;
(10) graphite heater, deposition precast body are well cut along contact surface, promptly obtain density 1.6-1.8g/cm
3Carbon/carbon compound material, and carbon/carbon compound material further detected, processes, obtain product.
5. method as claimed in claim 4 is characterized in that, described porous preform be shaped as annular, disc or bulk.
6. method as claimed in claim 4 is characterized in that, described heating power supply is resistive heating or induction heating.
7. a kind of according to claim 1 liquid precursor atomizing prepares the method for carbon/carbon compound material, it is characterized in that,
(1) prepare precast body, will have porous carbon felt, carbon cloth, and 2D or 3D carbon fiber knit system become certain size and shape;
(2) prepare graphite heater and annex thereof; According to precast body and the size of keeping for mist attitude precursor heating space; Confirm the size and the size of graphite heater; The material of graphite heater adopts commercially available common graphite, prepares a certain size and shape lagging material according to reaction chamber space size simultaneously, the protection body of heater;
(3) lagging material, graphite heater and precast body are put into reactor drum in order, guarantee that precast body one side closely contacts with the heating element hot face, form the high-temperature zone, guarantee that heating fully;
(4) with condenser cover also sealing on reactor drum, start oil-sealed rotary pump, the reactor drum air is evacuated to negative pressure, stop vacuum pump, fill in reactor drum through protection gas inlet then and protect gas N
2To a normal atmosphere, open the air outlet, and the flow that guarantees protection gas be the 10-40 liter/hour, start condenser cooling water;
(5) start heating power supply, through ruhmkorff coil heating graphite heater, heat-processed makes the temperature of its high-temperature zone rise to 900 ℃ through the temperature of the inboard high-temperature zone of thermocouple measurement porous preform;
(6) in reactor drum, spray mist attitude presoma through liquid precursor make up system and atomisation unit, through the concentration of the gas inside the atomisation unit controlling reactor;
(7) keep precast body high-temperature zone temperature at 900 ℃-1350 ℃, spraying continuously, deposition reaction 2-8 hour, and according to timely adjustment of precursor concentration in the reaction chamber and additional kerosene;
(8) stop atomisation unit successively earlier, stop heating power supply again, be cooled to room temperature after, stop shielding gas N
2And condenser cooling water;
(9) furnace cooling is opened condensing surface to room temperature, takes out graphite heater and fine and close carbon/carbon compound material successively;
(10) graphite heater and carbon/carbon compound material are cut along contact surface, and carbon/carbon compound material is further detected, processes, obtain the finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105168833A CN102010219B (en) | 2010-10-22 | 2010-10-22 | Method for preparing carbon/carbon composite material by liquid precursor atomization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105168833A CN102010219B (en) | 2010-10-22 | 2010-10-22 | Method for preparing carbon/carbon composite material by liquid precursor atomization |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102010219A CN102010219A (en) | 2011-04-13 |
| CN102010219B true CN102010219B (en) | 2012-11-28 |
Family
ID=43840576
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105168833A Expired - Fee Related CN102010219B (en) | 2010-10-22 | 2010-10-22 | Method for preparing carbon/carbon composite material by liquid precursor atomization |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102010219B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1736947A (en) * | 2005-07-18 | 2006-02-22 | 西安交通大学 | Method for preparing carbon/carbon composite material |
| CN1766153A (en) * | 2005-11-07 | 2006-05-03 | 西安交通大学 | Method for quick-speed preparing carbon/carbon composite material using heat gradient chemical gas phase infiltration |
-
2010
- 2010-10-22 CN CN2010105168833A patent/CN102010219B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1736947A (en) * | 2005-07-18 | 2006-02-22 | 西安交通大学 | Method for preparing carbon/carbon composite material |
| CN1766153A (en) * | 2005-11-07 | 2006-05-03 | 西安交通大学 | Method for quick-speed preparing carbon/carbon composite material using heat gradient chemical gas phase infiltration |
Non-Patent Citations (3)
| Title |
|---|
| Jiping Wang et al.A rapid fabrication of C/C composites by a thermal gradient chemical vapor infiltration method with vaporized kerosene as a precursor.《Materials Chemistry and Physics》.2007,第101卷(第1期),第7-11页. * |
| 张永辉等.化学液相气化渗透法制备炭/炭复合材料研究的进展.《硅酸盐学报》.2007,第35卷(第3期),第389-394页. * |
| 张永辉等.煤油蒸气为前驱体热梯度CVI法制备C/C复合材料.《新型炭材料》.2010,第25卷(第2期),第141-145页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102010219A (en) | 2011-04-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100370055C (en) | Method for quick-speed preparing carbon/carbon composite material using heat gradient chemical gas phase infiltration | |
| CN101456580B (en) | Method for preparing stannic oxide nano wire | |
| CN105925961A (en) | Laser chemical vapor deposition device for rapidly preparing multibasic oxide thin film | |
| CN103193498A (en) | Narrow flow induction coupling chemical vapor deposition (CVD) densification method for rapidly preparing carbon/carbon composite material crucible | |
| CN101357854A (en) | Postprocessing method for reducing thermal conductivity of ceramic heat barrier coating | |
| CN104451606A (en) | Fast vapor phase deposition thickening method of carbon/carbon composite material | |
| CN1328215C (en) | Method for preparing carbon/carbon composite material | |
| CN104446585B (en) | The method that batch quickly prepares high-density carbon/carbon composite material | |
| Igumenov et al. | Thermal barrier coatings on gas turbine blades: Chemical vapor deposition | |
| CN105016760A (en) | Preparation method for ultra-high-temperature ceramic modified C/C composite material | |
| CN105481477A (en) | Preparation method of graphite/SiC composite material | |
| CN104775103A (en) | Method for preparing ZrC coating | |
| Weber et al. | Deposition mechanisms of thick lanthanum zirconate coatings by spray pyrolysis | |
| KR101494237B1 (en) | Hybrid type isothermal-thermal gradient Chemical Vapor Infilteration(H-CVI) for Carbon-carbon composite manufacturing | |
| CN107265416A (en) | The preparation method of pyrolytic boron nitride material | |
| CN102010219B (en) | Method for preparing carbon/carbon composite material by liquid precursor atomization | |
| CN101077823A (en) | Gasifier | |
| US20030160044A1 (en) | High efficiency, oxidation resistant radio frequency susceptor | |
| CN101157565A (en) | Novel process for preparing charcoal/charcoal component by rapid chemical liquid-phase vaporization osmosis method | |
| CN112695266A (en) | Suspension, preparation method of coating and thermal barrier coating | |
| CN202380085U (en) | Gas purge system in LPCVD (low-pressure chemical vapor deposition) process chambers | |
| US20110253040A1 (en) | Apparatus For Forming Composite Membrane With Porous Coating Layer | |
| CN203373423U (en) | Equipment for preparing thin films and spraying patterns through spray combustion | |
| CN213835530U (en) | Solid-state source bottle | |
| CN213507160U (en) | Thermal barrier coating device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20121128 Termination date: 20151022 |
|
| EXPY | Termination of patent right or utility model |