CN104498891A - Carbon/carbon composite component chemical vapor infiltration device - Google Patents
Carbon/carbon composite component chemical vapor infiltration device Download PDFInfo
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- CN104498891A CN104498891A CN201410675591.2A CN201410675591A CN104498891A CN 104498891 A CN104498891 A CN 104498891A CN 201410675591 A CN201410675591 A CN 201410675591A CN 104498891 A CN104498891 A CN 104498891A
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Abstract
The invention brings forward a carbon/carbon composite component chemical vapor infiltration device and aims to provide a device for solving problems of low reactant gas utilization rate and low infiltration efficiency existing by chemical vapor infiltration in the prior art. The invention is realized by the following technical scheme: a gas mixing and preheating device for primary control of reactant gas diversion direction and a temperature sensor for monitoring preheating temperature of reactant gas are arranged below a deep gas-mixing and outgassing device connected with a sealed infiltration chamber; the regulated and controlled reactant gas enters a gas mixing and preheating device from the bottom of a chemical vapor deposition furnace body through a gas supply device, and a controller automatically regulates electric power on a heater to obtain required preheating temperature; and the preheated reactant gas enters the sealed infiltration chamber and passes through a porous graphite liner plate to infiltrate through a composite preform placed inside the sealed infiltration chamber, and chemical vapor infiltration is performed under constant values by pressure control of a furnace pressure controller and temperature control of a temperature control sensor.
Description
Technical field
The present invention relates to a kind of chemical vapor deposition stove preparation facilities of field of compound material.
Background technology
Carbon/carbon composite is a kind of carbon fiber reinforced carbon matrix composite, its electronic configuration based on carbon atom uniqueness and its feature such as graphite-like structure and good biocompatibility, be considered to desirable electro-conductive material, high temperature sandwich, functional materials and biomaterial, Aeronautics and Astronautics, biology and multiple civil area can be widely used in.The multiple preparation method of matrix material all has a high expensive problem, as conventional isothermal CVI technique, the fine and close time needs hundreds of even over thousands of hour, cycle is long, cost is high, operation of equipment is difficult, cause goods cost to remain high, this point seriously constrains the further application and development of this material.Chemical vapour deposition is the mode by chemical reaction, utilize the various energy such as heating, plasma excitation or optical radiation, in reactor, make the chemical substance of gaseous state or steam condition in gas phase or gas-solid interface, form the technology of solid deposited thing through chemical reaction.Chemical vapor infiltration (CVI) technique adopted in recent years is the extension of traditional chemical vapour deposition (CVD) technique, make gaseous substance (CH4, C3H6 etc.) the carbon fiber surface of heating or near generation chemical reaction, to migrate in composite preform deposition and obtain pyrolytic carbon matrix.In CVI technique density process, pyrolytic carbon take Carbon fibe as core growth, along with the carrying out of deposition, makes whole composite preform become the material entities of high-strength a, Gao Mo.The weak point of prior art chemical vapor infiltration technique is, densification rate is low, and preparation cycle is long, and production efficiency is very low, cost is high.Unavoidably there is the residual porosity of 10-15% in matrix material, affects mechanical property and the antioxidant property of matrix material.Prepare carbon/carbon composite processing condition such as the factors such as the specific surface area of temperature, pressure, unstripped gas C/H ratio, gas residence time and base substrate hole by CVI technique and have significant impact to base substrate microcell gas phase composition.
There are problems in the chemical vapor deposition stove of field of compound material, wherein leaking gas in process furnace etc. in the installation of furnace lining, electrical heating element and charcoal source gas exists much hidden danger.Be 200910093946.6 in Chinese Patent Application No., publication number a kind of high-performance carbon-based composite material slewing disclosed in CN101671188A is oozed in long-pending current-controlled method, and equipment used is exported by gas flow control device, gas mixer, gas preheating unit and gas and oozed long-pending furnace pressure device four part and forms.Principle of work composite preform is positioned over equipment to ooze long-pending indoor, is heated to temperature required, and the gas mixture that flow by a certain percentage passes into one or more reactant gasess enters and oozes long-pending indoor, and controls to carry out chemical vapor infiltration under pressure and amasss.The weak point that aforesaid method exists is: 1, gas preheating unit place is without automatically adjustable calorifier and monitor temperature sensor, cannot monitor and carry out the preheating temperature of regulating and controlling reactant gases, insufficient preheating will cause reactant gases cracking incomplete, greatly reduces the utilization ratio of reactant gases and finally oozes long-pending speed; 2, reactant gases returns behind primary heater unit top, and last bunchy enters composite preform and oozes long-pending indoor after being flowed out by surrounding air outlet bottom primary heater unit, reactant gases can not well be disperseed in primary heater unit, and pre-heat effect is not good; 3, when sheet material class A of geometric unitA is placed in device disclosed in the method and carries out oozing long-pending, because sheet material class A of geometric unitA airtightly oozes product space relatively with oozing cannot to be formed between long-pending device, the utilization ratio of reactant gases will be greatly reduced, increase the difficulty that system pressure controls, significantly reduce and ooze long-pending speed.
Summary of the invention
The object of the invention is for above-mentioned existing methodical weak point, a kind of reactant gases is provided to mix more abundant, even, pre-heat effect can be ensured, reach preset temperature, the abundant cracking of realization response gas, improve reactant gases utilization ratio, the carbon/carbon composite component chemical vapor infiltration that the best oozes long-pending efficiency can be obtained and amass device.With solve the reactant gases utilization ratio that prior art chemical vapor infiltration accumulates in lower, ooze the not high problem of long-pending efficiency.
Above-mentioned purpose of the present invention can be achieved by the following technical programs: a kind of carbon/carbon composite component chemical vapor infiltration amasss device, comprise the gas supply device 1 being communicated with chemical vapor deposition stove body 6 from bottom of furnace body, the furnace pressure control device 2 of gas supply device 1 is communicated with by steam line, be arranged on the mixed gas in chemical vapor deposition stove body furnace chamber and primary heater unit 3, the degree of depth is mixed gas and air-out apparatus 4 and is closed and oozes long-pending room 5, it is characterized in that: close and ooze long-pending room 5 degree of depth that is connected and mix gas and air-out apparatus 4, the degree of depth is mixed gas and is provided with one-level below air-out apparatus 4 and coordinates liner plate with holes to control mixed gas and the primary heater unit 3 in reactant gases water conservancy diversion direction, the temperature probe 3-5 monitoring reactant gases temperature is provided with in mixed gas and primary heater unit 3, gas supply device 1, furnace pressure control device 2 and mixed gas are electrically connected controller 7 with primary heater unit 3, reactant gases preheating temperature is monitored by preheating temperature probe 3-5, and carry out regulable control by controller 7, reactant gases through regulable control enters mixed gas by gas supply device 1 from the chemical vapor deposition stove body 6 furnace bottom inlet mouth 6-11 after vacuumizing to carry out mixing and preheating with primary heater unit 3, controller 7 is according to the information of temperature probe 3-5, and the electric power on automatic regulation heating device 3-4 obtains the preheating temperature needed, preheating reactant gases penetration depth mixes gas and air-out apparatus 4 is further mixed and disperses, reactant gases after overmulling gas and primary heater unit 3 enter formed by ring-shaped graphite cylinder 5-1, porous graphite liner plate 5-2, composite preform 5-4, graphite cover plate 5-6 closedly ooze long-pending room 5, infiltrate through through porous graphite liner plate 5-2 the composite preform 5-4 being placed on and closing and ooze in long-pending room 5, under furnace pressure control device 2 pressure-controlling and the temperature controlled definite value of temperature-control senser 6-14, carry out chemical vapor infiltration amass.
The present invention has following beneficial effect compared to prior art.
The present invention by increasing the temperature probe of monitoring reactant gases temperature in mixed gas and primary heater unit, by the calorifier of adjustable electric power, the temperature needed is obtained via the electric power on controller process temperature probe information on control panel and automatic regulation heating device, and increase one-level again and mix gas and air-out apparatus, make the mixing of reactant gases more fully, evenly, pre-heat effect can be ensured, reach preset temperature, the abundant cracking of realization response gas, improve reactant gases utilization ratio, the best can be obtained and ooze long-pending efficiency.
The present invention can carry out the long-pending gas and vapor permeation of chemical vapor infiltration and primary heater unit to being formed the closed carbon/carbon composite component oozing product space.It make the blending dispersion of gas evenly, flow in order, preheating temperature is fully controlled, then the directed long-pending indoor of oozing closed that import are oozed long-pending, improve the utilization ratio of reactant gases and ooze long-pending speed.Not only can improve carbon yield, reduction can infused composite precast body pore dimension, and can effectively prevent pitch from being extruded outside spiracular slit by the gas that pyrolysis produces, thus substantially increases efficiency of densification.
The present invention by increasing the temperature probe of monitoring reactant gases temperature in mixed gas and primary heater unit, the calorifier of the adjustable electric power of device, obtains the temperature needed via the electric power on controller process temperature probe information on control panel and automatic regulation heating device.Mixed gas and primary heater unit can make reactant gases preheating abundant, reach preset temperature, the abundant cracking of realization response gas, improve reactant gases utilization ratio, can obtain best densification rate.
The present invention mixed gas be provided with one-level above primary heater unit and coordinate liner plate with holes to control mixed gas and the air-out apparatus in reactant gases water conservancy diversion direction, accurately can control the water conservancy diversion direction of reactant gases, make simultaneously reactant gases further the degree of depth fully mix, dispersed, ensure that volumetric concentration is more homogeneous, pre-heat effect is more remarkable.
The present invention adopt ring-shaped graphite cylinder, porous graphite plate, graphite cover plate to form close ooze long-pending room, sealing effectiveness is better; Adopt hyperchannel deposition gas-path, even flow field, without deposition dead angle, deposition effect is good.Greatly improve the utilization ratio of reactant gases, higher densification rate can be obtained.
The invention solves prior art reactant gases pre-heat effect in primary heater unit not good, be difficult to reach preset temperature, abundant cracking cannot be realized, the closed problem of oozing product space can not be formed.Adopt the present invention that deposition cycle can be made significantly to shorten.
Accompanying drawing explanation
What Fig. 1 carbon/carbon composite component of the present invention chemical vapor infiltration amassed device analyses and observe organigram.
Fig. 2 is that the mixed gas of Fig. 1 and primary heater unit, the degree of depth mix gas and air-out apparatus structure for amplifying schematic diagram.
Fig. 3 is Fig. 1 porous graphite liner plate enlarged diagram.
In figure: 1 gas supply device, 1-1 first control valve, 1-2 first-class gauge 1,1-3 second control valve, 1-4 second gauge, 1-5 first control valve pickup wire, 1-6 first flow flowmeter sensor line, 1-7 second control valve pickup wire, 1-8 second flowmeter transducer line, 1-9 first via gas, 1-10 second road gas; 2 furnace pressure control devices, 2-1 first absolute pressure meter, 2-2 second absolute pressure meter 2,2-3 the 3rd absolute pressure meter, 2-4-vacuum pumping hardware, 2-5 first absolute pressure flowmeter sensor line, 2-6 second absolute pressure flowmeter sensor line, 2-7 the 3rd absolute pressure flowmeter sensor line, 2-8 vacuum pumping hardware pickup wire; 3 mixed gas and primary heater units, 3-1 graphite retaining ring, 3-2 pore, 3-3 porous graphite plate, 3-4 calorifier, 3-5 preheating temperature probe, 3-6 temperature probe line, 3-7 calorifier pickup wire; 4 degree of depth mix gas and air-out apparatus, 4-1 airslide lower plate, 4-2 air slot, 4-3 ventilating pit, 4-4 gas port, 4-5 airslide upper plate; 5 close ooze long-pending room, 5-1 ring-shaped graphite cylinder, 5-2 porous graphite liner plate, the little gas port of 5-3,5-4 composite preform, the large gas port of 5-5,5-6--graphite cover plate; 6 chemical vapor deposition stove bodies, 6-1 top carbon felt, 6-2 top graphite cover, 6-3 ruhmkorff coil, 6-4 furnace wall carbon felt, 6-5 graphite heater, 6-6 viewing window graphite tube, 6-7 monitoring sensor graphite tube, 6-8 graphite platen, graphite cake bottom 6-9,6-10 furnace bottom carbon felt, 6-11 furnace bottom inlet mouth, 6-12 high alumina brick, 6-13 production well, 6-14 temperature-control senser, 6-15 monitoring sensor; 7 controllers.
Specific embodiment mode
Consult Fig. 1-Fig. 3.In embodiment described below, the chemical vapor deposition stove that carbon/carbon composite component chemical vapor infiltration amasss device mixes gas and air-out apparatus 4 primarily of gas supply device 1, furnace pressure control device 2, mixed gas and primary heater unit 3, the degree of depth, closedly oozes long-pending room 5, chemical vapor deposition stove body 6 and totally six most ofly to form.Wherein, gas supply device 1 is communicated with chemical vapor deposition stove body 6 from bottom of furnace body, furnace pressure control device 2 is communicated with gas supply device 1 by steam line, and mixed gas and primary heater unit 3, the degree of depth are mixed gas and air-out apparatus 4 and closedly oozed long-pending room 5 and be arranged in chemical vapor deposition stove body furnace chamber.
Close and ooze long-pending room 5 degree of depth that is connected and mix gas and air-out apparatus 4, the degree of depth is mixed gas and is provided with one-level below air-out apparatus 4 and coordinates liner plate with holes to control mixed gas and the primary heater unit 3 in reactant gases water conservancy diversion direction, is provided with the temperature probe 3-5 monitoring reactant gases temperature in mixed gas and primary heater unit 3; Gas supply device 1, furnace pressure control device 2 and mixed gas are electrically connected controller 7 with primary heater unit 3; Reactant gases preheating temperature is monitored by preheating temperature probe 3-5, and carry out regulable control by controller 7, reactant gases through regulable control enters mixed gas by gas supply device 1 from the chemical vapor deposition stove body 6 furnace bottom inlet mouth 6-11 after vacuumizing to carry out mixing and preheating with primary heater unit 3, controller 7 is according to the information of temperature probe 3-5, and the electric power on automatic regulation heating device 3-4 obtains the preheating temperature needed; Preheating reactant gases penetration depth mixes gas and air-out apparatus 4 is further mixed and disperses, enter formed by ring-shaped graphite cylinder 5-1, porous graphite liner plate 5-2, composite preform 5-4, graphite cover plate 5-6 closedly ooze long-pending room 5, infiltrate through through porous graphite liner plate 5-2 the composite preform 5-4 being placed on and closing and ooze in long-pending room 5, under furnace pressure control device 2 pressure-controlling and the temperature controlled definite value of temperature-control senser 6-14, carry out chemical vapor infiltration amass.
Gas supply device 1 comprises: be connected to the first control valve 1-1 of gas supply device 1 gas path pipe first via gas 1-9 and first-class gauge 1-2, be connected to the second road gas 1-10 upper second control valve 1-3 and second gauge 1-4, first control valve 1-1 and first-class gauge 1-2 connects, first control valve 1-1 passes through first flow flowmeter sensor line 1-6 connection control device 7 by the first control valve pickup wire 1-5 connection control device 7, first-class gauge 1-2; Second control valve 1-3 and second gauge 1-4 connects, and the second control valve 1-3 passes through second flowmeter transducer line 1-8 connection control device 7 by the second control valve pickup wire 1-7 connection control device 7, second gauge 1-4.Above-mentioned under meter level is arranged on the front end being positioned at corresponding control valve, and for the size of measurement gas flow, under meter control valve is used for adjusting gas flow size.Controller carries out Dynamic comparison according to the gas flow size monitored and acquisition target gas flow value, obtains target gas flow value by the opening degree of adjusting control valve.
Furnace pressure control device 2 comprises: be connected to the first absolute pressure meter 2-1 on vacuum pumping hardware 2-4, second absolute pressure meter 2-2 and the 3rd absolute pressure meter 2-3 be connected on gas supply device 1 gas path pipe, and vacuum pumping hardware 2-4, first absolute pressure meter 2-1, second absolute pressure meter 2-2, 3rd absolute pressure meter 2-3 is connected respectively the first absolute pressure flowmeter sensor line 2-5 on controller 7, second absolute pressure flowmeter sensor line 2-6, vacuum pumping hardware pickup wire 2-8 and the 3rd absolute pressure flowmeter sensor line 2-7.First absolute pressure meter 2-1 is positioned at the side upper end of chemical vapor deposition stove body 6, the front end of vacuum pumping hardware 2-4, and the first absolute pressure meter 2-1 monitors the pressure of vacuum pumping hardware 2-4 front end; Second absolute pressure meter 2-2, near chemical vapor deposition stove body 6, is arranged in same level with the first absolute pressure meter 2-1, and the second absolute pressure meter 2-2 reflects chemical vapor deposition stove body 6 and closes the pressure oozing cavity between long-pending room 5; 3rd absolute pressure meter 2-3 is arranged on furnace bottom inlet mouth 6-11 lower end, for monitoring the pressure closed and ooze in long-pending room 5.Second absolute pressure meter 2-2, vacuum pumping hardware 2-4 are connected with controller 7 respectively by the second absolute pressure flowmeter sensor line 2-6, vacuum pumping hardware pickup wire 2-8, by the changing conditions of the force value of the second absolute pressure meter of display on controller 7, the opening degree of controller 7 regulating and controlling vacuum pumping hardware 2-4 is used to make the pressure-stabilisation of the second absolute pressure meter in setup pressure value.
Mixed gas and primary heater unit 3 comprise: porous graphite plate 3-3, the calorifier 3-4 and the preheating temperature probe 3-5 that are shaped with pore 3-2, porous graphite plate 3-3 is layered in the framework of calorifier 3-4 by the graphite retaining ring 3-1 separated around plate end, preheating temperature probe 3-5 is arranged between stacked porous graphite plate 3-3 space, is electrically connected controller 7 by temperature probe line 3-6 and calorifier pickup wire 3-7.The power adjustable of calorifier, the situation according to preheating temperature can carry out regulable control on the control panel.Porous graphite plate 3-3 is used for mixed gas and ventilation, can placement of multiple layers, and separate with graphite retaining ring 3-1 each other, be guarantee pre-heat effect, the pore 3-2 on adjacent porous graphite cake 3-3 should stagger mutually simultaneously.Reactant gases enters mixed gas and primary heater unit 3 by furnace bottom inlet mouth 6-11, reactant gases temperature is monitored by preheating temperature probe 3-5, and carry out regulable control by controller 7, controller 7 can process the information of preheating temperature probe 3-5, electric power on automatic regulation heating device 3-4 obtains the preheating temperature needed, until reactant gases leaves mixed gas and primary heater unit 3.Gas after overmulling gas and primary heater unit enter formed by ring-shaped graphite cylinder, porous graphite liner plate, composite preform, graphite cover plate closedly ooze long-pending room, air-flow by composite preform, carries out oozing long-pending via large gas port and little gas port directed flow in composite preform inside.
The described degree of depth mixes gas and air-out apparatus 4 comprises: connect firmly the airslide upper plate 4-5 on mixed gas and primary heater unit 3 upper port and airslide lower plate 4-1, airslide upper plate 4-5 plate body is shaped with ventilating pit 4-3 and gas port 4-4, between airslide lower plate 4-1 and airslide upper plate 4-5, forms air slot 4-2.Enter air slot 4-2 through the gas of overmulling gas after primary heater unit 3 by gas port 4-4 to carry out the degree of depth once again and mix and disperse, finally entered to close by ventilating pit 4-3 and ooze in long-pending room 5,6 are evenly distributed and measure-alike air slot 4-2.
Close and ooze long-pending room 5 and comprise: separate layer is stacked in the porous graphite liner plate 5-2 in ring-shaped graphite cylinder 5-1 cylindrical shell, and be positioned over ring-shaped graphite cylinder 5-2 graphite cover plate 5-6 topmost, the plate body of porous graphite liner plate 5-2 is shaped with the little gas port 5-3 that the large gas port 5-5 around center is symmetrically uniformly distributed arrangement, and composite preform 5-4 is placed on to close and oozes on the porous graphite liner plate 5-2 of long-pending room 5.
Chemical vapor deposition stove body 6 comprises: the graphite heater 6-5 sealed by the top graphite cover 6-2 being shaped with production well 6-13, at graphite heater 6-5, top graphite cover 6-2, bottom graphite cake 6-9 outside surface is coated with furnace wall carbon felt 6-4 respectively, top carbon felt 6-1, furnace bottom carbon felt 6-10, top carbon felt 6-1, furnace bottom carbon felt 6-10 is all tightly connected with furnace wall carbon felt 6-4, Tan Zhan6-1 upper end, top is provided with graphite platen 6-8 and by graphite platen 6-8, the viewing window graphite tube 6-6 of top carbon felt 6-1 and top graphite cover 6-2 and monitoring sensor graphite tube 6-7, monitoring sensor 6-15 is arranged in the cylindrical shell of graphite tube 6-7, ruhmkorff coil 6-3 is installed between furnace wall carbon felt 6-4 and the furnace wall of chemical vapor deposition stove body 6, chemical vapor deposition stove body 6 bottom part down is provided with the temperature-control senser 6-14 of the furnace bottom inlet mouth 6-11 at high alumina brick 6-12, furnace bottom carbon felt 6-10 and graphite cake 6-9 center in turn, and temperature-control senser 6-14 is electrically connected controller 7.
The principle of work of equipment is positioned over by composite preform to close to ooze long-pending indoor, be heated to preset temperature, pass into one or more reactant gasess through gas supply device flow by a certain percentage to carry out mixing and preheating with primary heater unit through mixed gas, penetration depth mixes gas and air-out apparatus is further mixed and disperses subsequently, with after penetrate into close through porous graphite liner plate and ooze long-pending indoor, and by furnace pressure control device, pressure-controlling is carried out chemical vapor infiltration under certain definite value and amasss.Concrete implementation step comprises:
(1) shove charge: put into by composite preform 5-4 on the porous graphite liner plate 5-2 of chemical vapor deposition stove 6, installs ring-shaped graphite cylinder 5-1, covers graphite cover plate 5-6, is formed to close to ooze long-pending room 5;
(2) also leak check situation is vacuumized: open vacuum pumping hardware 2-4, chemical vapor deposition stove 6 is vacuumized, discharge the air in chemical vapor deposition stove 6, the pressure being evacuated to the second absolute pressure meter 2-2 is 500Pa ~ 1000Pa, stopping vacuumizes, and checks that the pressure change of chemical vapor deposition stove 6 is to judge leakage situation;
(3) energising heats up and heats: energising intensification is heated to preset temperature, and being evacuated to 500Pa ~ 1000Pa simultaneously, preset temperature reaches predetermined temperature range respectively for closed temperature-control senser 5-14 and two the monitoring sensor 6-15 oozing furnace temperature temperature field in long-pending room 5 of monitoring and stablizes and is as the criterion.
(4) reactant gases (Sweet natural gas and propane) is passed into: flow by a certain percentage passes into Sweet natural gas and propane respectively in the gas circuit of gas supply device 1, under meter (1-2, 1-4) for the size of measurement gas flow, control valve (1-1, 1-3) for adjusting gas flow, control valve 1-1, under meter 1-2 and control valve 1-3, under meter 1-4 is by respective pickup wire 1-5, 1-6 and 1-7, 1-8 is connected with controller 7, controller 7 carries out Dynamic comparison according to the gas flow size monitored and acquisition target gas flow value, by regulating corresponding control valve 1-1, the opening degree of 1-3 obtains target gas flow value.
(5) the mixing and preheating of reactant gases (Sweet natural gas and propane): the reactant gases after gas supply device 1 imports mixed gas by furnace bottom inlet mouth 6-11 and mixes with primary heater unit 3, preheating, mix the adjustable calorifier 3-4 of electric power being configured with preheating temperature probe 3-5 and the preheating reactant gases of monitoring reactant gases temperature in gas and primary heater unit 3, preheating temperature probe 3-5 and calorifier 3-4 is by temperature probe line 3-6, calorifier pickup wire 3-7 is connected with controller 7, controller 7 can obtain the information of preheating temperature probe 3-5, controller 7 carrys out the electric power of regulation heating device 3-4 to reach the preheating temperature of needs according to the information of the preheating temperature probe 3-5 obtained, calorifier 3-4 is independently graphite heater.
Reactant gases mixed gas with carry out the mixing of short period of time, preheating in primary heater unit 3 after, then the degree of depth entering the adjacent side of being located thereon fast mixes gas and air-out apparatus 4, the air slot 4-2 that the gas port 4-4 that reactant gases is mixed in gas and air-out apparatus 4 by the degree of depth is evenly distributed by Decentralized Pull in six, mix further in air slot 4-2 reaction gases, disperse, then infiltrate through through porous graphite liner plate 5-2 the composite preform 5-4 being placed on and closing and ooze in long-pending room 5, carry out chemical vapor infiltration and amass.
The porous graphite plate 3-3 mixed in gas and primary heater unit 3 is used for mixed gas and ventilation, and thickness of slab is 20mm, and place four layers altogether, the height for the graphite retaining ring 3-1 located is 32mm, and the pore 3-2 on porous graphite plate 3-3 is Φ 11mm; That the degree of depth mixes ventilating pit 4-3 in gas and air-out apparatus 4 is Φ 10mm.The width of air slot 4-2 is 10mm, is highly 10mm, and the thickness of airslide 4-5 upper plate is 20mm.
(6) control of furnace pressure: close and ooze the reactant gases of long-pending room 5 or the production well 6-13 of waste gas on the graphite cover 6-2 of top is discharged by vacuum pumping hardware 2-4, furnace pressure carries out regulable control by furnace pressure control device 2, in the pressure of the second absolute pressure 2-2 for technology controlling and process pressure.
(7) blowing out: after chemical vapor infiltration amasss and reaches the scheduled time, stops passing into reactant gases, stops vacuumizing, and stop electrified regulation, come out of the stove when chemical vapor deposition stove is chilled to below 100 DEG C.
According to the present invention, component can be made to obtain homogeneous pyrolytic carbon structure, improve utilization ratio and the densification rate of reactant gases, be described further below by embodiment 1.
Embodiment 1:
(1) shove charge: by the porous graphite liner plate 5-2 in the horizontally mounted chemical vapor deposition stove 6 of 20 composite preforms (specification is 200mm × 200mm × 16mm) 5-4, being placed on by ring-shaped graphite cylinder 5-1 overlays on porous graphite liner plate 5-2, coping stone inky cap plate 5-6, on ring-shaped graphite cylinder 5-1, is formed to close and oozes long-pending room 5;
The thickness of porous graphite liner plate is 30mm, and large gas port 5-5 is 260mm, and little gas port 5-3 is 13mm.
The thickness of graphite cover plate 5-6 is 40mm, and the height of ring-shaped graphite cylinder is 300mm, thickness is 30mm.
(2) vacuumize also leak check situation: vacuumize chemical vapor deposition stove 6, the pressure being evacuated to the second absolute pressure meter 2-2 is 500Pa, stops vacuumizing, check that the pressure of chemical vapor deposition stove 6 is without considerable change;
(3) energising heats up and heats: energising intensification is heated to 1050 DEG C, and to be evacuated to the second absolute pressure meter pressure 2-2 be 1KPa simultaneously, treat that temperature-control senser 6-14 reaches and is stabilized in 1050 DEG C, the temperature of other two monitoring sensor 6-15 is respectively 1048 DEG C, 1048 DEG C and stablizes.
(4) reactant gases (Sweet natural gas and propane) is passed into: first via gas 1-9, the second road gas pass into Sweet natural gas and propane respectively, gas discharge is 10L/min, the volume ratio of Sweet natural gas/propane is 10:1, the flow of Sweet natural gas and propane carries out regulable control, to obtain required flow respectively by the first control valve 1-1 in gas supply device 1, first-class gauge 1-2 and the second control valve, second gauge.
(5) mixing of reactant gases and preheating: Sweet natural gas flows into mixed gas with propane by furnace bottom inlet mouth 6-11 and mixes with primary heater unit 3, heating, the preheating temperature of both gas mixtures is by the preheating temperature probe 3-5 and the common regulable control of electric power adjustable calorifier 3-4 that are configured in monitor temperature in mixed gas and primary heater unit, then both gas mixtures flow rapidly into the adjacent degree of depth by pore 3-2 and mix gas and mix further with air-out apparatus 4, dispersion, then infiltrate through through porous graphite liner plate 5-2 the composite preform 5-4 being placed on and closing and ooze in long-pending room 5, carry out chemical vapor infiltration to amass.
The porous graphite plate 3-3 mixed in gas and primary heater unit 3 is used for mixed gas and ventilation, and thickness of slab is 20mm, and place four layers altogether, the height for the graphite retaining ring 3-1 located is 32mm, and the pore 3-2 on porous graphite plate 3-3 is Φ 11mm; That the degree of depth mixes ventilating pit 4-3 in gas and air-out apparatus 4 is Φ 10mm.The width of air slot 4-2 is 10mm, is highly 10mm, and the thickness of airslide 4-5 upper plate is 20mm.
(6) control of furnace pressure: close and ooze the reactant gases of long-pending room or the production well 6-13 of waste gas on the graphite cover 6-2 of top is discharged by vacuum pumping hardware 2-4, furnace pressure carries out regulable control by furnace pressure control device 3, and the pressure-controlling of absolute pressure meter 2 (2-2) is 2.5KPa.
(7) blowing out: after chemical vapor infiltration amasss 285h, stops passing into Sweet natural gas, propane, stops vacuumizing, and stop electrified regulation, come out of the stove when chemical vapor deposition stove is chilled to 90 DEG C.
By embodiment 1, the rough layer pyrolytic carbon of the final even structure obtained, mean density reaches 1.63g/cm3 ~ 1.70g/cm3.
Claims (10)
1. a carbon/carbon composite component chemical vapor infiltration amasss device, comprise the gas supply device (1) being communicated with chemical vapor deposition stove body (6) from bottom of furnace body, the furnace pressure control device (2) of gas supply device (1) is communicated with by steam line, to be arranged in chemical vapor deposition stove body furnace chamber mixed gas and the degree of depth of primary heater unit (3) mix gas and air-out apparatus (4) and closedly ooze long-pending room (5), it is characterized in that: the closed connected degree of depth in long-pending room (5) of oozing mixes gas and air-out apparatus (4), the degree of depth is mixed gas and air-out apparatus (4) below and is provided with one-level and coordinates liner plate with holes to control mixed gas and the primary heater unit (3) in reactant gases water conservancy diversion direction, the temperature probe (3-5) of monitoring reactant gases preheating temperature is provided with in mixed gas and primary heater unit, gas supply device (1), furnace pressure control device (2) and mixed gas are electrically connected controller (7) with primary heater unit (3), reactant gases temperature is monitored by temperature probe (3-5), and carry out regulable control by controller (7), reactant gases through regulable control enters mixed gas by gas supply device (1) from chemical vapor deposition stove body (6) the furnace bottom inlet mouth (6-11) after vacuumizing to carry out mixing and preheating with primary heater unit (3), controller (7) is according to the information of temperature probe (3-5), and the electric power on automatic regulation heating device (3-4) obtains the preheating temperature needed, preheating reactant gases penetration depth mixes gas and air-out apparatus (4) is further mixed and disperses, enter formed by ring-shaped graphite cylinder (5-1), porous graphite liner plate (5-2), composite preform (5-4), graphite cover plate (5-6) closedly ooze long-pending room (5), infiltrate through through porous graphite liner plate (5-2) composite preform (5-4) being placed on and closing and ooze in long-pending room (5), under furnace pressure control device (2) pressure-controlling and temperature-control senser (6-14) temperature controlled definite value, carry out chemical vapor infiltration amass.
2. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amasss device, it is characterized in that: gas supply device (1) comprising: the first control valve (1-1) and the first-class gauge (1-2) that are connected to gas supply device (1) gas path pipe first via gas (1-9), be connected to the second control valve (1-3) on the second road gas (1-10) and second gauge (1-4), first control valve (1-1) and first-class gauge (1-2) series connection, first control valve (1-1) is by the first control valve pickup wire (1-5) connection control device (7), first-class gauge (1-2) is by first flow flowmeter sensor line (1-6) connection control device (7), second control valve (1-3) and second gauge (1-4) series connection, second control valve (1-3) is by the second control valve pickup wire (1-7) connection control device (7), and second gauge (1-4) is by second flowmeter transducer line (1-8) connection control device (7).
3. carbon/carbon composite component chemical vapor infiltration as claimed in claim 2 amasss device, it is characterized in that: control valve, under meter are connected with controller by respective respective sensor line, above-mentioned under meter level is arranged on the front end being positioned at corresponding control valve, for the size of measurement gas flow, under meter control valve is used for adjusting gas flow.
4. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amasss device, it is characterized in that: controller carries out Dynamic comparison according to the gas flow size monitored and acquisition target gas flow value, obtains target gas flow value by the opening degree of adjusting control valve.
5. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amasss device, it is characterized in that: furnace pressure control device (2) comprising: be connected to the first absolute pressure meter (2-1) on vacuum pumping hardware (2-4), second absolute pressure meter (2-2) and the 3rd absolute pressure meter (2-3) be connected on gas supply device (1) gas path pipe, and vacuum pumping hardware (2-4), first absolute pressure meter (2-1), second absolute pressure meter (2-2), 3rd absolute pressure meter (2-3) is connected respectively the first absolute pressure flowmeter sensor line (2-5) on controller (7), second absolute pressure flowmeter sensor line (2-6), vacuum pumping hardware pickup wire (2-8) and the 3rd absolute pressure flowmeter sensor line (2-7).
6. carbon/carbon composite component chemical vapor infiltration as claimed in claim 5 amasss device, it is characterized in that: the first absolute pressure meter (2-1) is positioned at the side upper end of chemical vapor deposition stove body (6), the front end of vacuum pumping hardware (2-4), and the pressure of vacuum pumping hardware (2-4) front end monitored by the first absolute pressure meter (2-1); Second absolute pressure meter (2-2) is near chemical vapor deposition stove body (6), be arranged in same level with the first absolute pressure meter (2-1), the second absolute pressure meter (2-2) reflects chemical vapor deposition stove body (6) and closes the pressure oozing cavity between long-pending room (5); 3rd absolute pressure meter (2-3) is arranged on furnace bottom inlet mouth (6-11) lower end, for monitoring the pressure closed and ooze in long-pending room (5).
7. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amasss device, it is characterized in that: mixed gas and primary heater unit (3) comprising: the porous graphite plate (3-3) being shaped with pore (3-2), calorifier (3-4) and preheating temperature probe (3-5), porous graphite plate (3-3) is layered in the framework of calorifier (3-4) by the graphite retaining ring (3-1) separated around plate end, preheating temperature probe (3-5) is arranged between stacked porous graphite plate (3-3) space, controller (7) is electrically connected by temperature probe line (3-6) and calorifier pickup wire (3-7).
8. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amasss device, it is characterized in that: the described degree of depth mixes gas and air-out apparatus (4) comprising: connect firmly the airslide upper plate (4-5) on mixed gas and primary heater unit (3) upper port and airslide lower plate (4-1), airslide upper plate (4-5) plate body is shaped with ventilating pit (4-3) and gas port (4-4), between airslide lower plate (4-1) and airslide upper plate (4-5), forms air slot (4-2); Enter air slot (4-2) through the gas of overmulling gas after primary heater unit (3) by gas port (4-4) to carry out the degree of depth once again and mix and disperse, finally entered to close by ventilating pit (4-3) and ooze in long-pending room (5).
9. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amasss device, it is characterized in that: close and ooze long-pending room (5) and comprising: separate layer is stacked in the porous graphite liner plate (5-2) in ring-shaped graphite cylinder (5-1) cylindrical shell, and be positioned over ring-shaped graphite cylinder (5-2) graphite cover plate (5-6) topmost, the plate body of porous graphite liner plate (5-2) is shaped with the little gas port (5-3) that the large gas port (5-5) around center is symmetrically uniformly distributed arrangement, composite preform (5-4) is placed on to close and oozes on the porous graphite liner plate (5-2) of long-pending room (5).
10. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amasss device, it is characterized in that: chemical vapor deposition stove body (6) comprising: the graphite heater (6-5) sealed by the top graphite cover (6-2) being shaped with production well (6-13), be coated on furnace wall carbon felt (6-4) that graphite heater (6-5) outside surface is sealed by top carbon felt (6-1), top carbon felt (6-1) upper end is provided with graphite platen (6-8) and passes through graphite platen (6-8), the viewing window graphite tube (6-6) of top carbon felt (6-1) and top graphite cover (6-2) and monitoring sensor are with graphite tube (6-7), monitoring sensor (6-15) is arranged in the cylindrical shell of graphite tube (6-7), the furnace bottom inlet mouth (6-1) 1 at the high alumina brick (6-12) that ruhmkorff coil (6-3) is connected in turn by chemical vapor deposition stove body (6) bottom part down, furnace bottom carbon felt (6-10) and graphite cake (6-9) center is electrically connected temperature-control senser (6-14).
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| CN105420686A (en) * | 2015-12-31 | 2016-03-23 | 清远先导材料有限公司 | Graphite depositing device for chemical vapor deposition furnace |
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| CN108558427A (en) * | 2018-05-22 | 2018-09-21 | 中南大学 | A method of preparing even density carbon/carbon composite tablet using confinement reactor batch |
| CN110241402A (en) * | 2019-07-08 | 2019-09-17 | 山东大学 | Chemical gaseous phase uniform deposition furnace |
| CN111574237A (en) * | 2020-05-22 | 2020-08-25 | 中南大学 | Oversized carbon/carbon composite material sheet and equipment for preparing same |
| CN112553604A (en) * | 2020-12-18 | 2021-03-26 | 上海骐杰碳素材料有限公司 | Continuous chemical vapor deposition furnace and working method thereof |
| CN112570189A (en) * | 2020-12-18 | 2021-03-30 | 上海骐杰碳素材料有限公司 | Continuous thermal spraying deposition furnace and working method thereof |
| CN113106428A (en) * | 2021-04-07 | 2021-07-13 | 锦州同创真空冶金科技有限公司 | Vacuum induction chemical vapor deposition furnace |
| CN113683436A (en) * | 2021-08-27 | 2021-11-23 | 清华大学 | Air inlet assembly, vapor deposition device and preparation method of composite material of vapor deposition device |
| CN113683436B (en) * | 2021-08-27 | 2022-09-16 | 清华大学 | Air inlet assembly, vapor deposition device and preparation method of composite material of vapor deposition device |
| CN115094402A (en) * | 2022-06-24 | 2022-09-23 | 清华大学 | Vertical double-temperature-zone-double-channel chemical vapor deposition equipment |
| CN115636685A (en) * | 2022-10-27 | 2023-01-24 | 上饶中昱新材料科技有限公司 | Method and system for preparing large-scale cylindrical carbon-carbon thermal field material in short period by using multiple material columns of CVI system |
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