CN100370055C - Method for quick-speed preparing carbon/carbon composite material using heat gradient chemical gas phase infiltration - Google Patents
Method for quick-speed preparing carbon/carbon composite material using heat gradient chemical gas phase infiltration Download PDFInfo
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- CN100370055C CN100370055C CNB2005100963062A CN200510096306A CN100370055C CN 100370055 C CN100370055 C CN 100370055C CN B2005100963062 A CNB2005100963062 A CN B2005100963062A CN 200510096306 A CN200510096306 A CN 200510096306A CN 100370055 C CN100370055 C CN 100370055C
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Abstract
The present invention discloses a rapid preparation method for C/C composite materials by thermal gradient chemical vapor infiltration. An upper independent graphite heating body and a lower independent graphite heating body are arranged in a thermal gradient chemical vapor infiltration device; the lower heating body is treated by boiling gasification of a liquid precursor and provides a carbon source with high activity for cracking reaction; a prefabricated body and the upper heating body are positioned above the liquid level of the precursor by a support stick and a supporting board containing holes, the prefabricated body is heated by the upper heating body, and thermal gradient is formed in the thickness direction of the upper heating body; after being convected and diffusion diffused through a short path, the gasified carbon source enters the prefabricated body and prepares deposit carbon by cracking reaction; the deposit carbon deposits for 4 to 10 hours, and the prefabricated body can be densified into the C/C composite materials with the density of 1.6 to 1.8 g/cm<3>. The method has the advantages of simple needed equipment, easy regulation and control of technical parameters and great reduction of energy consumption, is suitable for rapid industrial production of disk-shaped C/C composite materials, various aeroplane C brake disks and the densification research and the preparation of other porous composite materials and has wide application prospects.
Description
Technical field
The present invention relates to a kind of quick preparation of matrix material, particularly a kind of is the method that the heat gradient chemical gaseous phase permeation of carbon source prepares carbon/carbon (C/C) matrix material fast with the liquid precursor vapour.
Background technology
Carbon/carbon (C/C) matrix material has high specific strength, high specific stiffness, high temperature and keeps high strength down, the designability of good ablation property, frictional behaviour and good thermal shock resistance energy and matrix material, at space flight, aviation field, especially wide application prospect is arranged as the aircraft brake material.At present, (Chemical vapor infiltration is the main method of preparation C/C matrix material CVI) to the isothermal chemical vapor infiltration, though this technology has certain advantage, its weak point is preparation technology's excessive cycle, and utilization rate of raw materials is low.For this reason round the production efficiency that how to improve the C/C matrix material, reduce preparation cost, relevant scholar has carried out a large amount of research both at home and abroad, isothermal pressure gradient CVI, thermal gradient CVI, pulse CV I, forced-flow thermal gradient CVI have been developed, and chemical liquid phase gasification osmose process (Chemicalliquid-vaporized infiltration, CLVI, or be called as Film boiling CVI, method such as FBCVI).Wherein the densification rate of chemical liquid phase gasification osmose process is the highest, has shortened the time of preparation C/C matrix material greatly, has reduced preparation cost.
Existing CLVI method all is that graphite heater and the precast body (enhancing bodies such as carbon felt, carbon cloth or carbon fiber knit body) around it are immersed in the liquid precursor (carbon sources such as hexanaphthene, kerosene) fully, by the mode of induction heating or resistive heating, in the sizable thermal gradient of the inner generation of precast body.When precast body inboard temperature is enough high, make liquid precursor boiling, gasification and scission reaction take place to generate deposit carbon, with the reaction times prolongation, pass gradually laterally from the precast body inboard in the densification forward position, finishes 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.
Yet also there is certain defective in the CLVI method of announcing at present, mainly shows:
(1) forming being reflected in the ebullient liquid precursor of deposit carbon carries out, this process is influenced by hydromeehanics, gas-liquid two-phase flow, boiling heat transfer and complicated chemical reaction jointly, not only be difficult to give theoretically accurate the explanation and calculating, and realization and the control to processing parameter is also very difficult in the actually operating;
(2) to make liquid precursor in precast body, form gaseous film (being film boiling) and scission reaction generation deposit carbon, the huge heating power that needs has sufficiently high temperature to guarantee the precast body inboard, a large amount of wastes of electric energy had so both been caused, cause the liquid precursor acutely to seethe with excitement again, make it rapid consumption; And atmosphere pressures surpasses malleation in the reactor, has certain danger;
(3) in the deposition process, can not realize independence control, can not measure and control reactant (gas concentration, pressure) to preform temperatures.
Therefore be necessary to the CLVI further improvements in methods.
Summary of the invention
At the defective or the deficiency that exist in the above-mentioned existing CLVI method, the object of the present invention is to provide the method for the fast densified C/C matrix material of a kind of heat gradient chemical gaseous phase permeation, this method is applicable to disc C/C matrix material, and the industrialization of various airplane carbon brake discs is produced fast, and can reach: (1) shortens process cycle, prepares density and reach 1.6～1.8g/cm in the utmost point short period of time (4～10 hours)
3The C/C matrix material; (2) cut down the consumption of energy, further improve the utilization ratio of liquid precursor; (3) controllability, stability and the security of realization processing parameter (heating power, heat-up rate, reactant concn etc.).
Technical solution of the present invention is as follows:
A kind of heat gradient chemical gaseous phase permeation prepares the C/C composite process, adopt the heat gradient chemical gaseous phase permeation device, this device comprises reactor, condenser, vacuum system, the atmosphere protection system, heating system, temperature control system, the liquid precursor make up system, described liquid precursor is selected from kerosene, gasoline, diesel oil, hexanaphthene is wherein a kind of, it is characterized in that: on this method adopts in device, the design of following two independent heating elements, be used for heating precast body and liquid precursor respectively, by support stick and supporting plate precast body and liquid precursors are separated, not directly contact; Make the presoma ebullition, gasification by following heating element, form the very big gaseous carbon source of activity; By last heating element heating precast body, and form big thermal gradient, for the gaseous carbon source scission reaction and form RESEARCH OF PYROCARBON enough temperature are provided at its thickness direction.
The concrete preparation process of aforesaid method comprises the following steps:
(1) preparation precast body
To have porous carbon felt or carbon cloth or 2D carbon fiber knit body or 3D carbon fiber knit body is made certain size and shape as requested;
(2) preparation graphite heater and positioning attachment
According to the size of precast body, process the upper and lower cylinder graphite heater of certain size respectively, process one and have the even supporting plate in hole respectively, process several support sticks;
(3) will descend graphite heater, support stick, supporting plate, precast body and last graphite heater to put into reactor in order;
(4) in reactor, add liquid precursor by the liquid precursor make up system, make its liquid level be higher than heating element down, but be lower than the lower surface of supporting plate;
(5) with condenser cover also sealing on reactor, start oil-sealed rotary pump, air in the reactor is evacuated to below the 1kPa, stop vacuum pump, in reactor, fill shielding gas to a normal atmosphere by protection gas inlet then, open the air outlet, and guarantee that the flow of shielding gas is 10～40 liters/hour, start condenser cooling water;
(6) start heating power supply, heat upper and lower graphite heater simultaneously; Heat-processed makes its surface temperature rise to 1000 ℃～1300 ℃ by the surface temperature of thermopair 1 measurement precast body; Total depositing time is 4～10 hours, measures the liquid level height of judging liquid precursor in the reactor by thermopair 2 in this process, real-time additional liquid precursor in reactor;
(7) stop heating power supply successively, shielding gas and condenser cooling water;
(8) graphite heater, precast body and supporting plate in the taking-up;
(9) will go up graphite heater, precast body and supporting plate and cut, promptly obtain the fine and close density 1.6～1.8g/cm of being of precast body along contact surface
3The C/C matrix material, and this C/C matrix material further detected, processes, obtain the finished product.
In suitability for industrialized production, to use method of the present invention and prepare the C/C matrix material, its superiority is mainly reflected in:
(1) characteristics of essence of the present invention are that the precast body of carbon fiber knit body or carbon felt, carbon cloth or its combination was made density in 4～10 hours reach 1.6～1.8g/cm fast
3The C/C matrix material;
(2) great advantage of the existing CLVI technology of the present invention is: can be easy to realize the required technological temperature of deposit carbon reaction by the appropriate design to last heating element size dimension or type of heating;
(3) the present invention can be by the appropriate design to following heating element size or type of heating, the controllability of realization response gas concentration, pressure and other parameters;
(4) present device is simple, can adopt resistive heating or induction heating, can reduce facility investment significantly as adopting the resistive heating mode;
(5) the present invention can further save electric energy, and improves the liquid precursor utilization ratio;
(6) graphite heater of the present invention can reuse, by changing the preparation that the big I of heating element realizes the C/C matrix material of different size size.
Description of drawings
Fig. 1 (a) is that the present invention adopts induction heating to prepare the synoptic diagram of single-piece disc C/C composite device fast, and Fig. 1 (b) is the graphite supporting plate of device, and ratio can be done suitable convergent-divergent according to the actual requirements among the figure.
Symbol among the figure is expressed as respectively: cylinder graphite heater on 101; heating precast body upper surface; 102 precast bodies; 103 have the graphite supporting plate of uniform distribution aperture; be used for fixing precast body, its equally distributed aperture can make gaseous reactant enter precast body, 104 liquid precursor; 105 times cylinder graphite heaters; make the liquid precursor ebullition, gasification, for deposition reaction provides carbon source, 106 heat insulation propping materials; prevent that reactor bottom is overheated; 107 is the equally distributed 4 graphite small column support sticks of circumferential direction, precast body and last heating element is separated 108 reactors with liquid precursors; 109 ruhmkorff coils; 110 intermediate frequency induction heating power supplies, 111 condensers reenter reactor with unreacted gaseous carbon source cooling; 112 oil-sealed rotary pumps; 113 protection gas inlets, 114 reaction gas outlet, 115 and 116 is thermopair; be used for measuring the temperature on precast body surface and height, 117 liquid precursor deposits and the additional inlet of judgement liquid precursor liquid level respectively.
Fig. 2 is the graphite heater and the precast body design of the annular C/C matrix material of preparation.
Symbol among the figure is expressed as respectively: cylinder graphite heater on 201, heating precast body upper surface, 202 are used to heat the undersized cylinder graphite heater of precast body internal diameter, 203 have the graphite supporting plate of uniform distribution aperture, 204 liquid precursor, 205 times cylinder graphite heaters, 206 annular precast bodies, 207 is the equally distributed 4 graphite small column support sticks of circumferential direction, be used for supporting 203 with and top parts.
Below in conjunction with the embodiment that the principle and the contriver of accompanying drawing and technical scheme provides, the present invention is described in further detail.
Embodiment
The present invention has adopted a kind of and the diverse mentality of designing of forefathers' technology, adopt two independently heating element (following heating element and last heating element) realize the scission reaction of boiling, gasification and the gaseous reactant of liquid precursor respectively.
Below in conjunction with accompanying drawing 1, the detailed process for preparing monolithic C/C matrix material for the present invention is described below:
(1) prepare precast body 102, will have porous carbon felt, carbon cloth, and 2D or 3D carbon fiber knit system become certain size and shape;
(2) graphite heater 101, following graphite heater 105, graphite supporting plate 103 in the preparation, size according to precast body, determine the diameter of graphite heater, highly, the material of graphite heater adopts commercially available common graphite, prepare 4 graphite support sticks 107 simultaneously, the size of support stick can guarantee that steadily supporting (101～103) gets final product, and prepares lagging material 106;
(3) lagging material 106, following graphite heater 105, support stick 107, supporting plate 103, precast body 102 and last graphite heater 101 are put into reactor in order;
(4) in reactor 108, add liquid precursor 104 by liquid precursor make up system 117, guarantee that liquid level is higher than cylinder graphite heater down, but will be lower than the lower surface of graphite supporting plate 103;
(5) condenser 111 is placed on the reactor 108 and sealing, start oil-sealed rotary pump 112, air in the reactor is evacuated to certain negative pressure, stop vacuum pump, in reactor 108, fill protection gas to one normal atmosphere by protection gas inlet 113 then, open air outlet 114, and guarantee that the flow of protection gas is 10～40 liters/hour, start condenser cooling water 111;
(6) start medium frequency induction power supply 110, by ruhmkorff coil 109 heating graphite heaters (101,105), measure the porous preform surface temperature by thermopair 115, make surface temperature rise to 1000 ℃～1300 ℃, depositing time is 4～10 hours, measures the height of judging liquid precursor liquid level in the reactor by thermopair 116 in this process, real-time additional liquid precursor in reactor;
(7) stop induction heating power 110 successively, protection gas 113 and condenser cooling water 111;
(8) open condenser 111, take out graphite heater 101 and fine and close C/C matrix material 102 successively;
(9) graphite heater 101 and C/C matrix material 102 are cut along contact surface, and C/C matrix material 102 is further detected, processes, obtain the finished product.
In conjunction with the accompanying drawings 2, the graphite heater and the precast body specification that the present invention are prepared annular C/C matrix material are as follows:
For preparing annular C/C matrix material 206, the graphite supporting plate 203 heating precast bodies 206 of cylinder graphite heater 201 and uniform distribution aperture in the employing.Adopt the interior circle of the annular porous preform of a little cylinder graphite heater 202 heating simultaneously.Other processing step is identical with the description of above-mentioned preparation single-piece disc C/C matrix material.
The contriver provides following 2 embodiment, but the invention is not restricted to these embodiment.
Embodiment 1: according to technical scheme of the present invention, 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.It is as follows to adopt method of the present invention to prepare the concrete steps of disc C/C matrix material of single-piece:
(1) prepares precast body, the carbon felt is cut to Φ 100 * 10mm
3Size;
(2) prepare graphite heater, upper and lower graphite heater is processed as diameter of phi 100mm, thickness is respectively 130mm and 100mm, prepares to be of a size of Φ 100 * 15mm
3Disk is as supporting plate, and evenly bores several apertures (Φ 10mm) thereon, prepares 4 size Φ 15 * 100mm
3The graphite support stick, prepare heat insulating mattress (common alumina brick);
(3) alumina brick, following graphite heater, support stick, supporting plate, precast body and last graphite heater are put into reactor in order;
(4) in reactor, add kerosene by the liquid precursor make up system, guarantee that liquid level is higher than cylinder graphite heater down, but will be lower than the lower surface of supporting plate;
(5) with condenser cover also sealing on reactor, start oil-sealed rotary pump, air pressure in the reactor is evacuated to below the 1kPa, stop vacuum pump, in reactor, fill N by 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;
(6) start medium frequency induction power supply, ruhmkorff coil heats upper and lower graphite heater, measure the precast body surface temperature by thermopair 1, make surface temperature rise to 1050 ℃～1150 ℃, deposit 6 hours, measure the height of judging presoma liquid level in the reactor by thermopair 2 in this process, real-time additional kerosene in reactor;
(7) stop induction heating power, N successively
2And condenser cooling water;
(8) open condenser, graphite heater, precast body and supporting plate in the taking-up;
(9) will go up graphite heater, precast body and supporting plate and cut, and the C/C matrix material is further detected, processes, obtain the finished product along contact surface;
The mean density of the final carbon felt basic circle plate-like C/C matrix material that obtains is 1.65g/cm
3
Embodiment 2: according to technical scheme of the present invention, adopt the acupuncture one dimension carbon cloth precast body of preparation aeroplane brake discs, density is～0.5g/cm
3It is as follows to adopt method of the present invention to prepare the concrete steps of annular C/C matrix material of single-piece:
(1) prepares precast body, acupuncture one dimension carbon cloth is cut to external diameter Φ 140mm, internal diameter Φ 50mm, the annular size of high 20mm;
(2) prepare graphite heater, upper and lower graphite heater is processed as Φ 140 diameters, thickness is respectively 130mm and 100mm, prepares to be of a size of Φ 140 * 15mm
3Disk is as supporting plate, and evenly bores several apertures (Φ 10mm) thereon, prepares 4 size Φ 15 * 100mm
3The graphite support stick, prepare heat insulating mattress (common alumina brick); Increase simultaneously and be of a size of Φ 50 * 20mm
3Graphite heater be used to heat the interior ring of porous preform;
(3) alumina brick, following graphite heater, support stick, supporting plate, precast body, little heating element and last graphite heater are put into reactor in order;
(4) in reactor, add kerosene by the liquid precursor make up system, guarantee that liquid level is higher than cylinder graphite heater down, but will be lower than the lower surface of supporting plate;
(5) with condenser cover also sealing on reactor, start oil-sealed rotary pump, air pressure in the reactor is evacuated to below the 1kPa, stop vacuum pump, in reactor, fill N by 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;
(6) start medium frequency induction power supply, ruhmkorff coil heats upper and lower graphite heater, measure the precast body surface temperature by thermopair 1, make surface temperature rise to 1050 ℃～1150 ℃, deposit 8 hours, measure the height of judging presoma liquid level in the reactor by thermopair 2 in this process, real-time additional kerosene in reactor;
(7) stop induction heating power, N successively
2And condenser cooling water;
(8) open condenser, graphite heater, precast body and supporting plate in the taking-up;
(9) will go up graphite heater, precast body and supporting plate and cut, and the C/C matrix material is further detected, processes, obtain the finished product along contact surface;
The mean density of the final acupuncture one dimension carbon cloth basic circle plate-like C/C matrix material that obtains is 1.73g/cm
3
Claims (5)
1. a heat gradient chemical gaseous phase permeation prepares the C/C composite process, adopt the heat gradient chemical gaseous phase permeation device, this device comprises reactor, condenser, vacuum system, atmosphere protection system, heating system, temperature control system, liquid precursor make up system, it is wherein a kind of that described liquid precursor is selected from kerosene, gasoline, diesel oil, hexanaphthene, it is characterized in that this method adopts upper and lower independently two graphite heaters in device; Following heating element is realized the ebullition, gasification of liquid precursor, for scission reaction provides active very high carbon source; By support stick, contain the hole supporting plate precast body and last heating element be positioned to be positioned at presoma liquid level top, last heating element is used for heating precast body, and forms thermal gradient at its thickness direction; The carbon source of gasification enters precast body and scission reaction and generates deposit carbon through convection current, the diffusion of short path, deposits after 4～10 hours, and can be 1.6～1.8g/cm with the fine and close one-tenth of precast body density
3The C/C matrix material.
2. the method for claim 1 is characterized in that, the concrete preparation process of this method comprises the following steps:
(1) preparation precast body
To have porous carbon felt or carbon cloth or 2D carbon fiber knit body or 3D carbon fiber knit body is made certain size and shape as requested;
(2) preparation graphite heater and positioning attachment
According to the size of precast body, process the upper and lower cylinder graphite heater of certain size respectively, process one and have the even supporting plate in hole respectively, process several support sticks;
(3) will descend graphite heater, support stick, supporting plate, precast body and last graphite heater to put into reactor in order;
(4) in reactor, add liquid precursor by the liquid precursor make up system, make its liquid level be higher than heating element down, but be lower than the lower surface of supporting plate;
(5) with condenser cover also sealing on reactor, start oil-sealed rotary pump, air in the reactor is evacuated to below the 1kPa, stop vacuum pump, in reactor, fill shielding gas to a normal atmosphere by protection gas inlet then, open the air outlet, and guarantee that the flow of shielding gas is 10～40 liters/hour, start condenser cooling water;
(6) start heating power supply, heat upper and lower graphite heater simultaneously; Heat-processed makes its surface temperature rise to 1000 ℃～1300 ℃ by the surface temperature of thermopair 1 measurement precast body; Total depositing time is 4～10 hours, measures the liquid level height of judging liquid precursor in the reactor by thermopair 2 in this process, real-time additional liquid precursor in reactor;
(7) stop heating power supply successively, shielding gas and condenser cooling water;
(8) graphite heater, precast body and supporting plate in the taking-up;
(9) will go up graphite heater, precast body and supporting plate and cut, promptly obtain the fine and close density 1.6～1.8g/cm of being of precast body along contact surface
3The C/C matrix material, and this C/C matrix material further detected, processes, obtain the finished product.
3. method as claimed in claim 2 is characterized in that described shielding gas is selected from nitrogen or argon gas.
4. method as claimed in claim 2 is characterized in that, described precast body be shaped as annular or disc.
5. method as claimed in claim 2 is characterized in that, described heating power supply is resistive heating or induction heating.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010219B (en) * | 2010-10-22 | 2012-11-28 | 西安交通大学 | Method for preparing carbon/carbon composite material by liquid precursor atomization |
| CN103044056B (en) * | 2013-01-10 | 2014-08-13 | 湖南南方搏云新材料有限责任公司 | Technology and equipment for preparing C/C composite |
| CN103723729B (en) * | 2013-12-27 | 2015-04-22 | 黑龙江工程学院 | Preparation method of gradient activated carbon |
| CN107058941B (en) * | 2017-05-16 | 2019-05-03 | 重庆理工大学 | Infiltration method and device are expanded in the heating of gear surface vacuum induction |
| CN110016803B (en) * | 2019-04-04 | 2019-12-20 | 碳翁(北京)科技有限公司 | High-temperature-resistant electric heating fiber and application thereof |
| CN111348931B (en) * | 2020-03-26 | 2024-02-09 | 孚迪斯石油化工（葫芦岛）有限公司 | Annular carbon/carbon composite material gas phase permeation method |
| CN114134484B (en) * | 2021-11-28 | 2023-11-21 | 西北工业大学 | Vortex auxiliary system and method for preparing fiber reinforced composite material by chemical vapor infiltration method |
| CN113912408B (en) * | 2021-11-30 | 2023-04-25 | 甘肃新西北碳素科技有限公司 | Quick preparation method of aircraft brake disc |
| CN116283330A (en) * | 2022-10-19 | 2023-06-23 | 西北工业大学 | Preparation method of directional deposition heterogeneous CC composite material |
| CN115819101B (en) * | 2022-11-25 | 2023-07-21 | 湖南博云新材料股份有限公司 | Method for rapidly preparing carbon/carbon composite brake disc |
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| CN1377855A (en) * | 2002-04-30 | 2002-11-06 | 西安交通大学 | Process for preparing C/C composite material fastly using super critical fluid technology |
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| CN1377855A (en) * | 2002-04-30 | 2002-11-06 | 西安交通大学 | Process for preparing C/C composite material fastly using super critical fluid technology |
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| C/C多孔体的制备及其对C/C－SiC－Si复合材料的影响. 姜华等.陶瓷科学与艺术，第6期. 2003 * |
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