CN101798078B - Quick carbon deposition method of carbon/carbon material member - Google Patents
Quick carbon deposition method of carbon/carbon material member Download PDFInfo
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- CN101798078B CN101798078B CN2010101531245A CN201010153124A CN101798078B CN 101798078 B CN101798078 B CN 101798078B CN 2010101531245 A CN2010101531245 A CN 2010101531245A CN 201010153124 A CN201010153124 A CN 201010153124A CN 101798078 B CN101798078 B CN 101798078B
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Abstract
The invention provides a quick carbon deposition method of a carbon/carbon material member, which comprises the following steps: (1) putting a carbon fiber preform into a high-temperature graphitizing furnace for high-temperature pretreatment; (2) fixedly connecting the carbon fiber preform with a heating unit, and isolating the carbon fiber preform from the heating unit by an isolator; (3) putting the carbon fiber preform and the heating unit assembly into a deposition chamber, putting a thermocouple on the external surface of the carbon fiber preform, vacuumizing for eliminating atmosphere firstly, and then, introducing reaction gas; and (4) heating the heating unit, and carrying out vapor deposition of carbon for 20-200h to prepare the carbon/carbon material member once. In the method of the invention for preparing the carbon/carbon member, the thermocouple only needs to be put on the external surface of the member, thus the member does not need to be perforated in the process of preparation, and the integrity of the member can be kept. The method of the invention has short production cycle and low process cost, can realize the purpose of quick densification, and is suitable for large-scale production in batches.
Description
Technical field
The present invention relates to a kind of method of carbon/carbon material rapid shaping, particularly adopt the heavy carbon technique of temperature differential method gas phase to prepare the method for large size carbon/carbon material member fast.
Background technology
The method for densifying of carbon/carbon material promptly is to fill its hole with certain carbon base body, makes carbon fiber strengthen skeleton and reaches the technological process with high volume density by low volume density.Chemical vapor deposition (CVD) carbon and liquid impregnation carbonization are the densifying methods of widespread use.Wherein liquid impregnation carbonization carburizing tech exists equipment requirements height, quality of item problem of unstable, and the one, no matter impregnating equipment or carbonizing apparatus all need bigger capacity; The 2nd, no matter all there are problems such as the carbonization process goods are easy to crack, distortion in resin carbon or bitumencarb, there is the goods foreign matter content more simultaneously, the defective that work-ing life is short.Except liquid impregnation carbonization technology, the carbon/carbon compound material densification process also adopts gas phase to sink carbon technique, divide according to type of heating, pressure range, gas flow form or other modes, mainly contain soaking method CVD, temperature differential method CVD, pulse CV D, pressure differential method CVD etc.Isothermal CVD technology is the most frequently used in the gas-phase deposition, the simplest a kind of densifying method.The shape of product that this processing method is made be not subjected to condition restriction and in enormous quantities shove charge produce, technology is corresponding ripe, the production of suitable most of goods.But because bottleneck effect produces, need repeatedly blowing out in the technological process, the workpiece surface skinning machine is processed, adjust deposition position, process cycle is chronic, as the goods of producing higher density need reach 1000～1600 hours depositing time, causes cost high.And common temperature differential method CVD technical requirements thermopair inserts goods inside, and moves with the speed of 0.25～1mm/h, and this just need be in certain position perforating for the treatment of goods with the placement thermopair, thereby goods have been caused localized injury, has influenced its use.
Summary of the invention
The object of the present invention is to provide a kind of quick carbon deposition method of carbon/carbon material member, overcome the deficiency of existing densification technology, solve the problem that goods need punch in the existing quick CVI technology of temperature differential method.
Realize the technical scheme of the object of the invention: a kind of quick carbon deposition method of carbon/carbon material member, described prefabricated carbon fiber body is by the multilayer cloth lamination, or adopts acupuncture behind the lamination or sew up the fabric that all carbon cloths are coupled together; This method comprises the steps
(1) the prefabricated carbon fiber body is put into the high temperature graphitization stove and carry out the high temperature pre-treatment, the high temperature pretreatment temperature is 2000～2500 ℃, soaking time 1～3 hour;
(2) the pretreated prefabricated carbon fiber body of step (1) high temperature is fixedlyed connected with heating element, separate with isolated body between prefabricated carbon fiber body and the heating element;
(3) prefabricated carbon fiber body and the heating element subassembly that step (2) is obtained is positioned in the sediment chamber, and thermopair is put in the outer surface of prefabricated carbon fiber body; Vacuumize the eliminating atmosphere earlier, feed reactant gases malleation 0.1～5.0kPa to the sediment chamber again; Continue to feed in the sediment chamber reactant gases then, the control flow rate of reactive gas is 1～10m
3/ h;
(4) heating element heating when the deposition room temp reaches 600～1200 ℃, is pressed the speed continuation increase temperature of 1～10 ℃/h again, through the heavy carbon of 20～200h gas phase, stop heating and be cooled to room temperature, the supply of stopped reaction gas can disposable preparation volume density reach 1.3～1.8g/cm
3Carbon/carbon material member.
The quick carbon deposition method of aforesaid a kind of carbon/carbon material member, its described prefabricated carbon fiber body be shaped as hollow disc, hollow circuit cylinder or tabular, the volume density scope is 0.10～0.65g/cm
3
The quick carbon deposition method of aforesaid a kind of carbon/carbon material member, its described isolated body adopts kraft paper or flexible graphite paper.
The quick carbon deposition method of aforesaid a kind of carbon/carbon material member, its described heating element is graphite or carbon/carbon compound material.
The quick carbon deposition method of aforesaid a kind of carbon/carbon material member, its described heating element is realized heating in the mode of direct energising.
The quick carbon deposition method of aforesaid a kind of carbon/carbon material member, its described prefabricated carbon fiber body and heating element fixed form are bonding or binding of carbon rope or carbon fibre tow stitching.
The quick carbon deposition method of aforesaid a kind of carbon/carbon material member, its described reactant gases are methane or propane or propylene.
Effect of the present invention is:
(1) the invention solves that thermopair moves the problem that need punch in the quick CVI process of common temperature differential method on goods.Prepare carbon/carbon member method by the present invention, thermopair is put in external surface of structural member and gets final product, so member need not punch in the preparation process, and the integrity of energy retaining member.
(2) the present invention avoided the adhesion between precast body and the heating element, and process implementing is very easy by isolate kraft paper or flexible graphite paper between precast body and heating element.
(3) prepare carbon/carbon member method by the present invention, with short production cycle, the technology cost is low, can realize the purpose of quick densifying, is suitable for large size and batch process.
(4) visual precast body of the inventive method and end article density requirements, design heating curve and other heavy carbon processing parameter can accurately be controlled the goods final state.
(5) evidence, the carbon/carbon goods mechanical property excellence of this method preparation, porosity is low, is suitable for use as all kinds of solar heat protection, carrying, corrosion resistant member.
Description of drawings
Fig. 1 is that the quick carbon deposition method of carbon/carbon material member uses parts assembling synoptic diagram;
Among the figure: 1. top electrode; 2. heating element; 3. sealing coat; 4. prefabricated carbon fiber body; 5. thermopair; 6. lower electrode.
Embodiment
Be further described in detail below in conjunction with the quick carbon deposition method of specific embodiment a kind of carbon/carbon material member of the present invention.
Embodiment 1
(1) adopt PAN base 12k carbon fiber, prepare the prefabricated carbon fiber body of no latitude cloth screening tire needling structure mode, the prefabricated carbon fiber body is a hollow cylindrical, size Φ 600mm (external diameter) * Φ 540mm (internal diameter) * 800mm (highly), and initial density is 0.45g/cm
3
(2) the prefabricated carbon fiber body is put into the high temperature graphitization stove and carry out the high temperature pre-treatment, 2000 ℃ of high temperature pretreatment temperatures, soaking time 3h, its volume density is 0.425g/cm after the high temperature pre-treatment
3
(3) as shown in Figure 1, the prefabricated carbon fiber body 4 usefulness 6k carbon fibers that step (2) high temperature pre-treatment is intact are bundled on the heating element 2, isolate 3 with two-layer kraft paper between prefabricated carbon fiber body 4 and the heating element 2.Heating element processes with graphite material, is of a size of Φ 540mm (external diameter) * Φ 500mm (internal diameter) * 1000mm (highly).Heating element 2 installs top electrode 1 and lower electrode 6 up and down respectively additional, and top electrode 1 and lower electrode 6 also process with graphite material, is of a size of Φ 650mm * 50mm (thickness).
(4) prefabricated carbon fiber body and the heating element subassembly with step (3) places in the sediment chamber, and thermopair 5 is installed, and as shown in Figure 1, thermopair 5 is positioned at the outer surface of prefabricated carbon fiber body 1.Vacuumize the eliminating atmosphere earlier, after vacuum tightness reaches below the 30Pa, feed propane gas,, and keep 2m to malleation+4kPa
3The flow of/h constantly feeds propane gas in the sediment chamber.
(5) heat up for upper and lower electrifying electrodes, the heating element heating; After the deposition room temp reaches 850 ℃, speed by+4 ℃/h constantly increases temperature, through the 80 hours heavy carbon of gas phase, stop heating during temperature to 1170 ℃, be cooled to room temperature, the stop supplies propane gas is taken out the carbon/carbon material member that makes, its flat appearance, nothing are out of shape warpage, color and luster is even, no delamination splitting defective.The volume density of measuring member reaches 1.6g/cm
3
(1) adopt PAN base 6k carbon fiber, prepare the prefabricated carbon fiber body of no latitude cloth screening tire needling structure mode, the prefabricated carbon fiber body is a hollow cylindrical, is of a size of Φ 650mm (external diameter) * Φ 540mm (internal diameter) * 400mm (highly), and initial density is 0.46g/cm
3
(2) the prefabricated carbon fiber body is put into the high temperature graphitization stove and carry out the high temperature pre-treatment, 2200 ℃ of high temperature pretreatment temperatures are incubated 1 hour, and its volume density is 0.432g/cm after the high temperature pre-treatment
3
(3) as shown in Figure 1, the prefabricated carbon fiber body and function 12k carbon fiber that step (2) high temperature pre-treatment is intact is bundled on the heating element 2, and the flexible graphite paper 3 with 0.5mm thickness between prefabricated carbon fiber body 4 and the heating element 2 is isolated.Heating element processes with graphite material, is of a size of Φ 539mm (external diameter) * Φ 500mm (internal diameter) * 600mm (highly).Heating element 2 installs top electrode 1 and lower electrode 6 up and down respectively additional.Top electrode and lower electrode also process with graphite material, are of a size of Φ 650mm * 50mm (thickness).
(4) prefabricated carbon fiber body and the heating element subassembly with step (3) gained places in the sediment chamber, and thermopair 5 is installed, and as shown in Figure 1, thermopair 5 is positioned at the outer surface of prefabricated carbon fiber body 1.Vacuumize the eliminating atmosphere earlier, after vacuum tightness reaches below the 30Pa, feed methane gas,, keep 5m then to malleation+3kPa
3The flow of/h constantly feeds methane gas in the sediment chamber.
(5) heat up the heating element heating for top electrode 1 and lower electrode 6 energisings; When the deposition room temp reaches 1000 ℃, constantly increase temperature by the speed of+1 ℃/h again, through the heavy carbon of 200h gas phase, temperature to 1200 ℃ stops heating, is cooled to room temperature, stops to feed methane gas, takes out carbon/carbon material member.Defectives such as the distortionless distortion of this products appearance, layering, the volume density of measuring goods reaches 1.8g/cm
3
Embodiment 3
(1) adopt PAN base 6k carbon fiber, preparation plain weave cloth lamination structure, the prefabricated carbon fiber body is a tabular, is of a size of 800mm * 800mm * 50mm, initial density is 0.65g/cm
3
(2) the prefabricated carbon fiber body is put into the high temperature graphitization stove and carry out the high temperature pre-treatment, 2000 ℃ of high temperature pretreatment temperatures are incubated 2 hours, and its volume density is 0.63g/cm after the high temperature pre-treatment
3
(3) 0.5mm is thick flexible graphite paper is bonded on the heating element with resol, and then the prefabricated carbon fiber body and function resol that step (2) high temperature pre-treatment is intact is bonded on the flexible graphite paper.Heating element processes with graphite material, is of a size of 900mm * 900mm * 20mm.Heating element 2 installs top electrode 1 and lower electrode 6 up and down respectively additional.Top electrode and lower electrode also process with graphite material, are of a size of Φ 650mm * 50mm (thickness).
(4) prefabricated carbon fiber body and the heating element subassembly with step (3) gained places in the sediment chamber, and thermopair 5 is installed on the outer surface of prefabricated carbon fiber body 1.Vacuumize the eliminating atmosphere earlier, after vacuum tightness reaches below the 10Pa, feed methane gas,, and keep 1m to malleation 0.1kPa
3The flow of/h constantly feeds methane gas in the sediment chamber.
(5) heat up the heating element heating for top electrode 1 and lower electrode 6 energisings; When initial depositing temperature in the sediment chamber after 600 ℃, and constantly increase by the speed of 10 ℃/h, through the heavy carbon of 50h gas phase, take out the carbon/carbon material goods, defectives such as the distortionless distortion of this products appearance, layering.The volume density of measuring goods reaches 1.7g/cm
3
Embodiment 4
(1) adopt PAN base 12k carbon fiber, preparation plain weave cloth lamination structure, the prefabricated carbon fiber body is a tabular, is of a size of 800mm * 800mm * 20mm, initial density is 0.2g/cm
3
(2) the prefabricated carbon fiber body is put into the high temperature graphitization stove and carry out the high temperature pre-treatment, 2500 ℃ of high temperature pretreatment temperatures are incubated 1 hour, and its volume density is 0.18g/cm after the high temperature pre-treatment
3
(3) step (2) high temperature pre-treatment is intact prefabricated carbon fiber body and function 12k carbon fiber bundle is sewn on the heating element, isolates with kraft paper between prefabricated carbon fiber body 4 and the heating element 2.Heating element processes with carbon/carbon compound material, is of a size of 850mm * 850mm * 30mm.Heating element 2 installs top electrode 1 and lower electrode 6 up and down respectively additional.Top electrode and lower electrode also process with graphite material, are of a size of Φ 650mm * 50mm (thickness).
(4) prefabricated carbon fiber body and the heating element subassembly with step (3) gained places in the sediment chamber, and thermopair 5 is installed on the outer surface of prefabricated carbon fiber body 1.Vacuumize the eliminating atmosphere earlier, after vacuum tightness reaches below the 50Pa, feed propane gas,, and keep 10m to malleation 5kPa
3The flow of/h constantly feeds propane gas in the sediment chamber.
(5) heat up the heating element heating for top electrode 1 and lower electrode 6 energisings; When initial depositing temperature in the sediment chamber after 1200 ℃, and constantly increase by the speed of 1 ℃/h, through the heavy carbon of 40h gas phase, take out the carbon/carbon material goods, defectives such as the distortionless distortion of this products appearance, layering.The volume density of measuring goods reaches 1.8g/cm
3
The quick carbon deposition method of carbon/carbon material member of the present invention:
(1) the prefabricated carbon fiber body is by the multilayer cloth lamination, or adopts acupuncture behind the lamination or sew up the fabric that all carbon cloths are coupled together.The carbon cloth structure can be mat, various structure carbon cloth, no latitude cloth and other cloths.Can be as required, the size of control precast body finally exists circular hole, square hole, groove etc. to need the position of processing excision as goods, can directly cut on precast body, also can use the carbon cloth that has solid shape that weaves in advance.The shape of precast body can be hollow disc, hollow circuit cylinder, tabular, and its volume density scope is 0.10～0.65g/cm
3
(2) the prefabricated carbon fiber body is put into the high temperature graphitization stove and carry out the high temperature pre-treatment.High temperature pretreatment temperature scope is 2000～2500 ℃, soaking time 1～3h.
(3) the pretreated precast body of high temperature is fixedlyed connected with heating element.Use isolated body between fiber preform and the heating element, separate, to prevent the adhesion in technological process of precast body and heating element as kraft paper or flexible graphite paper.Heating element is realized heating in the mode of direct energising.Heating element can be graphite, C/C or high temperature alloy; Fixed form can be that binding of bonding, carbon rope or carbon fibre tow are sewed up.
(4) adopt constant pressure-fired method.Reactant gases is fed in the sediment chamber, make it to keep the constant slight positive pressure state.Reactive gas species comprises hydrocarbon gas such as methane, propane, propylene, and its initial depositing temperature is all different with pressure range.The constant pressure span of control is+0.1～5.0kPa.
(5) temperature thermocouple is positioned at the prefabricated carbon fiber external surface, does not move, and temperature improves constantly according to specific heating curve, causing the continuous deposition from the component inside to the outside, thereby realizes quick sedimentation process.Initial depositing temperature maintains 600～1200 ℃, and specific heating curve is meant: the speed by+1～10 ℃/h improves heavy carbon temperature.
(6) constantly feed reactant gases by certain flow, its flow is looked in the sediment chamber precast body total mass and required final densities and is determined and adjust.Through the heavy carbon of the gas phase of 20～200h, can disposable preparation volume density reach 1.3～1.8g/cm
3Carbon/carbon goods.
Claims (3)
1. the quick carbon deposition method of a carbon/carbon material member, described prefabricated carbon fiber body is by the multilayer cloth lamination, or adopts acupuncture behind the lamination or sew up the fabric that all carbon cloths are coupled together; It is characterized in that: this method comprises the steps
(1) the prefabricated carbon fiber body is put into the high temperature graphitization stove and carry out the high temperature pre-treatment, the high temperature pretreatment temperature is 2000～2500 ℃, soaking time 1～3 hour;
(2) the pretreated prefabricated carbon fiber body of step (1) high temperature is fixedlyed connected with heating element, separate with isolated body between prefabricated carbon fiber body and the heating element; Described heating element is graphite or carbon/carbon compound material; Described isolated body adopts kraft paper or flexible graphite paper;
(3) prefabricated carbon fiber body and the heating element subassembly that step (2) is obtained is positioned in the sediment chamber, and thermopair is put in the outer surface of prefabricated carbon fiber body; Vacuumize the eliminating atmosphere earlier, feed reactant gases malleation 0.1～5.0kPa to the sediment chamber again; Continue to feed in the sediment chamber reactant gases then, the control flow rate of reactive gas is 1～10m
3/ h; Described prefabricated carbon fiber body and heating element fixed form are bonding or binding of carbon rope or carbon fibre tow stitching;
(4) heating element heating when the deposition room temp reaches 600～1200 ℃, is pressed the speed continuation increase temperature of 1～10 ℃/h again, through the heavy carbon of 20～200h gas phase, stop heating and be cooled to room temperature, the supply of stopped reaction gas can disposable preparation volume density reach 1.3～1.8g/cm
3Carbon/carbon material member; Described heating element is realized heating in the mode of direct energising.
2. the quick carbon deposition method of a kind of carbon/carbon material member according to claim 1 is characterized in that: described prefabricated carbon fiber body be shaped as hollow disc, hollow circuit cylinder or tabular, the volume density scope is 0.10～0.65g/cm
3
3. the quick carbon deposition method of a kind of carbon/carbon material member according to claim 1, it is characterized in that: described reactant gases is methane or propane or propylene.
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| CN102030554B (en) * | 2010-11-02 | 2013-07-31 | 西安超码科技有限公司 | Method for compacting carbon/carbon composite material by using natural gas mixture CVI (Chemical Vapor Infiltration) |
| CN102211765B (en) * | 2011-03-28 | 2013-06-26 | 航天材料及工艺研究所 | Method for preparing carbon material with high heat conductivity by densifying gaps of graphite paper |
| CN102320853B (en) * | 2011-08-24 | 2013-07-03 | 中南大学 | Preparation method of carbon-based composite cathode material with highly-oriented emission characteristic |
| CN104561846B (en) * | 2014-12-24 | 2016-11-23 | 中南大学 | A kind of preparation method of continuous lod carbon/carbon-niobium composite |
| CN105714250A (en) * | 2016-02-19 | 2016-06-29 | 西安理工大学 | Preparation method of N-doped amorphous carbon film resistive random access memory |
| CN108220913B (en) * | 2018-01-24 | 2020-01-14 | 航天睿特碳材料有限公司 | Rapid low-cost CVD (chemical vapor deposition) densification method for carbon/carbon composite material |
| CN116283330B (en) * | 2022-10-19 | 2024-06-07 | 西北工业大学 | Preparation method of directional deposition heterogeneous CC composite material |
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| CN101157563A (en) * | 2007-09-13 | 2008-04-09 | 北京航空航天大学 | Process for preparing charcoal/charcoal component by electrothermy orienting infiltration |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101157563A (en) * | 2007-09-13 | 2008-04-09 | 北京航空航天大学 | Process for preparing charcoal/charcoal component by electrothermy orienting infiltration |
Non-Patent Citations (1)
| Title |
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| 张福勤等.炭/炭复合材料可石墨化性能的研究.《矿冶工程》.2001,第21卷(第1期),第59-61页. * |
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Application publication date: 20100811 Assignee: Space flight Rui Te carbon material company limited Assignor: Aerospace Material & Technology Inst. Contract record no.: 2014990000324 Denomination of invention: Quick carbon deposition method of carbon/carbon material member Granted publication date: 20111109 License type: Exclusive License Record date: 20140521 |
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