CN104498891B - Carbon/carbon composite component chemical vapor infiltration device - Google Patents
Carbon/carbon composite component chemical vapor infiltration device Download PDFInfo
- Publication number
- CN104498891B CN104498891B CN201410675591.2A CN201410675591A CN104498891B CN 104498891 B CN104498891 B CN 104498891B CN 201410675591 A CN201410675591 A CN 201410675591A CN 104498891 B CN104498891 B CN 104498891B
- Authority
- CN
- China
- Prior art keywords
- gas
- chemical vapor
- carbon
- graphite
- preheating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
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, and it is based on the unique electronics row of carbon atom
The features such as cloth and its graphite-like structure and good biocompatibility, is it is considered to be preferable conductive material, high temperature composite junction
Structure material, functional material and biomaterial, can be widely applied to Aeronautics and Astronautics, biological and multiple civil area.Composite
Multiple preparation methods all have a high expensive problem, the isothermal cvi technique such as commonly used, and the fine and close time needs hundreds of or even over thousands of little
When, cycle length, high cost, equipment operation are difficult, lead to goods cost to remain high, this point seriously constrains entering of this material
One step application and development.Chemical vapor deposition is by way of chemical reaction, using heating, plasma excitation or light radiation
Etc. the various energy, make the chemical substance of gaseous state or steam condition through chemical reaction shape in reactor in gas phase or gas-solid interface
Become the technology of solid deposited thing.Chemical vapor infiltration (cvi) technique adopting in recent years is traditional chemical vapor deposition (cvd)
The extension of technique, make gaseous substance (ch4, c3h6 etc.) heating carbon fiber surface or near produce chemical reaction, migrate to
In composite preform, deposition obtains being pyrolyzed carbon matrix.During cvi technique density, pyrolytic carbon is given birth to Carbon fibe for core
Long, with the carrying out of deposition, make whole composite preform become high-strength, Gao Mo material entities.Prior art
Learn gas-phase permeation technique and be disadvantageous in that, densification rate is low, long preparation period, production efficiency is very low, high cost.Compound
Unavoidably there is the residual porosity of 10-15%, the mechanical property of impact composite and antioxygenic property in material.Use cvi work
Skill prepares carbon/carbon composite process conditions such as temperature, pressure, unstripped gas c/h ratio, gas residence time and base substrate hole
The factors such as specific surface area have significant impact to base substrate microcell gas phase group Chengdu.
There are problems in the chemical vapor deposition stove of field of compound material, wherein furnace lining, the installation of heating and
There are many hidden danger in the gas leakage etc. in heating furnace of charcoal source gas.It is 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, used
Equipment by the output of gas flow control device, gas mixer, gas preheating unit and gas and oozes long-pending furnace pressure device four
Part forms.Operation principle is composite preform to be positioned over equipment ooze long-pending interior, is heated to temperature required, by certain than
The gaseous mixture that the flow of example is passed through one or more reacting gas enters to infiltrate long-pending interior, and controls and changed under pressure
Gas phase is oozed long-pending.Said method exists and is disadvantageous in that: 1, no adjustable heating element and prison automatically at gas preheating unit
Testing temperature sensor is it is impossible to monitoring and carry out controlling to adjust the preheating temperature of reacting gas, insufficient warm-up will leading to react
Gas cracking not exclusively, greatly reduces the utilization rate of reacting gas and finally oozes long-pending speed；2nd, reacting gas is to preheating device
Return behind top, last bunchy oozes long-pending interior by entering composite preform after the outflow of preheating device bottom surrounding gas outlet,
Reacting gas can not be disperseed in preheating device well, and pre-heat effect is not good；3rd, sheet material class component is placed on the method public affairs
When carrying out in the device opened oozing long-pending, because sheet material class component relative airtight oozes product space with oozing cannot be formed between long-pending device, it will
Greatly reduce the utilization rate of reacting gas, increase the difficulty that system pressure controls, be greatly lowered and ooze long-pending speed.
Content of the invention
The purpose of the present invention is the weak point for above-mentioned existing method, provides a kind of reacting gas mixing more to fill
Point, uniformly, both can guarantee that pre-heat effect, reached predetermined temperature, realized the abundant cracking of reacting gas, and improved reacting gas and utilize
Rate, can obtain the long-pending device of carbon/carbon composite component chemical vapor infiltration most preferably oozing long-pending efficiency.To solve prior art chemistry gas
Mutually ooze that the reacting gas utilization rate accumulating in is relatively low, ooze long-pending inefficient problem.
The above-mentioned purpose of the present invention can be achieved by the following technical programs: a kind of carbon/carbon composite componentization
Learn gas phase and ooze long-pending device, including the gas supply device 1 from bottom of furnace body connection chemical vapor deposition stove body 6, by air supply pipe
Furnace pressure control device 2, the mixed gas being arranged in chemical vapor deposition stove body furnace chamber and pre- hot charging that road connects gas supply device 1
Put 3, depth mix gas ooze long-pending room 5 with air-out apparatus 4 and closing it is characterised in that: closing is oozed long-pending room 5 and is connected the mixed gas of depth and giving vent to anger
Device 4, depth mix be provided with below gas and air-out apparatus 4 one-level cooperation liner plate with holes control the mixed gas in reacting gas water conservancy diversion direction with
Preheating device 3, is provided with, in mixed gas and preheating device 3, the temperature transducer 3-5 monitoring reacting gas temperature；Gas supply device 1,
Furnace pressure control device 2 and mixed gas electrically connect controller 7 with preheating device 3；Reacting gas preheating temperature is by preheating temperature transducer
3-5 is monitored, and is adjusted controlling by controller 7, and the reacting gas of adjusted control passes through gas supply device 1 from taking out
Chemical vapor deposition stove body 6 furnace bottom air inlet 6-11 after vacuum is entered mixed gas and is mixed with preheating device 3 and preheat, and controls
Device 7 obtains, according to the information of temperature transducer 3-5, the electrical power automatically adjusting on heating element 3-4, the preheating temperature needing；Preheating
Reacting gas is entered the mixed gas of depth and is further mixed with air-out apparatus 4 and disperses, through the reaction after overmulling gas and preheating device 3
The envelope that gas entrance is formed by ring-shaped graphite cylinder 5-1, porous graphite liner plate 5-2, composite preform 5-4, graphite cover plate 5-6
Close and ooze long-pending room 5, infiltrate through to be placed on through porous graphite liner plate 5-2 and close the composite preform 5-4 oozing in long-pending room 5,
Carry out chemical vapor infiltration under furnace pressure control device 2 Stress control and the temperature controlled definite value of temperature-control senser 6-14 to amass.
The present invention has the advantages that compared to prior art.
The present invention passes through to increase the temperature transducer of monitoring reacting gas temperature in mixed gas with preheating device, by adjustable
The heating element of economize on electricity power, processes temperature transducer information via controller on control panel and automatically adjusts the electricity on heating element
Power obtains the temperature needing, and is further added by one-level and mixes gas and air-out apparatus so that being more fully mixed, all of reacting gas
Even, both can guarantee that pre-heat effect, reached predetermined temperature, realized the abundant cracking of reacting gas, improve reacting gas utilization rate, can
Obtain and most preferably ooze long-pending efficiency.
The present invention can carry out chemical vapor infiltration and amass to the carbon/carbon composite component oozing product space that cannot form closing
Gas mixing and preheating device.It makes the mixing of gas be uniformly dispersed, flow in order, preheating temperature controlled fully, then
The long-pending interior of oozing that orientation imports closing is oozed long-pending, improves the utilization rate of reacting gas and oozes long-pending speed.Carbon residue not only can be improved
Rate, reduction can infused composite precast body pore-size, and can effectively prevent pitch be pyrolyzed generation gas extrusion gas
Outside hole, thus substantially increasing efficiency of densification.
The present invention passes through to increase the temperature transducer of monitoring reacting gas temperature in mixed gas with preheating device, and device is adjustable
The heating element of economize on electricity power, processes temperature transducer information via controller on control panel and automatically adjusts the electricity on heating element
Power obtains the temperature needing.Mixed gas and preheating device enable to reacting gas preheating fully, reach predetermined temperature, realize anti-
Answer the abundant cracking of gas, improve reacting gas utilization rate, optimal densification rate can be obtained.
The present invention is provided with one-level cooperation liner plate with holes above mixed gas with preheating device and controls reacting gas water conservancy diversion direction
Mixed gas and air-out apparatus, can make reacting gas further depth fill with the water conservancy diversion direction of precise control reacting gas simultaneously
Point mixing, dispersed it is ensured that volumetric concentration is more homogeneous, pre-heat effect is more significantly.
The present invention using ring-shaped graphite cylinder, porous graphite plate, graphite cover plate composition closing ooze long-pending room, sealing effectiveness is relatively
Good；Using multichannel deposition gas-path, even flow field, no deposit dead angle, deposition effect is good.Greatly improve the profit of reacting gas
With rate, higher densification rate can be obtained.
The present invention solves that prior art reacting gas pre-heat effect in preheating device is good, the pre- constant temperature of difficult to reach
Spend, cannot realize fully cracking, can not be formed the problem oozing product space of closing.Deposition cycle can be made significantly using the present invention
Shorten.
Brief description
Fig. 1 carbon/carbon composite of the present invention component chemical vapor infiltration amasss the section view organigram of device.
Fig. 2 is mixed gas and the mixed gas of preheating device, depth and the air-out apparatus mplifying structure schematic diagram of Fig. 1.
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 flowmeter 1,1-3 second control valve, 1-4 second
Flowmeter, 1-5 the first control valve pickup wire, 1-6 first flowmeter pickup wire, 1-7 the second control valve pickup wire, 1-8
Second flowmeter pickup wire, 1-9 first via gas, 1-10 the second road gas；2 furnace pressure control devices, 2-1 the first absolute pressure meter,
2-2 the second absolute pressure meter 2,2-3 the 3rd absolute pressure meter, 2-4 vacuum pumping hardware, 2-5 the 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 preheating device,
3-1 graphite locating ring, 3-2 pore, 3-3 porous graphite plate, 3-4 heating element, 3-5 preheats temperature transducer, 3-6 temperature transducer
Line, 3-7 heating element pickup wire；4 depth mix gas and air-out apparatus, 4-1 airslide lower plate, 4-2 air slot, 4-3 passage, 4-
4 gas ports, 4-5 airslide upper plate；Long-pending room is oozed in 5 closings, 5-1 ring-shaped graphite cylinder, 5-2 porous graphite liner plate, the little gas port of 5-3,
5-4 composite preform, the big 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 induction coil, 6-4 furnace wall carbon felt, 6-5 graphite heater, 6-6 observation window graphite tube, 6-7 monitoring sensing
Device graphite tube, 6-8 graphite platen, 6-9 bottom graphite cake, 6-10 furnace bottom carbon felt, 6-11 furnace bottom air inlet, 6-12 high-alumina brick,
6-13 venthole, 6-14 temperature-control senser, 6-15 monitors sensor；7 controllers.
Specific embodiment mode
Refering to Fig. 1-Fig. 3.In embodiment described below, carbon/carbon composite component chemical vapor infiltration amasss device
Chemical vapor deposition stove is mainly mixed gas and is gone out by gas supply device 1, furnace pressure control device 2, mixed gas and preheating device 3, depth
Device of air 4, closing ooze long-pending room 5, chemical vapor deposition stove body 6 totally six most of composition.Wherein, gas supply device 1 is from body of heater
Bottom connects chemical vapor deposition stove body 6, and furnace pressure control device 2 connects gas supply device 1 by steam line, mixed gas with advance
Thermal 3, depth mix gas and air-out apparatus 4 and closing is oozed long-pending room 5 and is arranged in chemical vapor deposition stove body furnace chamber.
Closing is oozed long-pending room 5 depth that is connected and is mixed gas and air-out apparatus 4, and depth is mixed and is provided with one-level below gas and air-out apparatus 4 and joins
Crossed belt hole liner plate controls mixed gas and the preheating device 3 in reacting gas water conservancy diversion direction, is provided with monitoring reaction in mixed gas and preheating device 3
The temperature transducer 3-5 of gas temperature；Gas supply device 1, furnace pressure control device 2 and mixed gas electrically connect control with preheating device 3
Device 7 processed；Reacting gas preheating temperature is monitored by preheating temperature transducer 3-5, and is adjusted controlling by controller 7, warp
Adjust the reacting gas controlling and pass through chemical vapor deposition stove body 6 furnace bottom air inlet 6- after vacuumizing for the gas supply device 1
11 enter mixed gas is mixed with preheating device 3 and is preheated, and controller 7, according to the information of temperature transducer 3-5, automatically adjusts and sends out
Electrical power on hot device 3-4 obtains the preheating temperature needing；Preheating reacting gas enters the mixed gas of depth and is entered one with air-out apparatus 4
Step mixing and dispersion, enter by ring-shaped graphite cylinder 5-1, porous graphite liner plate 5-2, composite preform 5-4, graphite cover plate 5-
Long-pending room 5 is oozed in the closing of 6 formation, infiltrates through to be placed on through porous graphite liner plate 5-2 and closes the composite precast oozing in long-pending room 5
Body 5-4, carries out chemical vapor infiltration under furnace pressure control device 2 Stress control and the temperature controlled definite value of temperature-control senser 6-14
Long-pending.
Gas supply device 1 includes: is connected to first control of gas supply device 1 gas path pipe first via gas 1-9
Valve 1-1 and first flowmeter 1-2, are connected to upper second control valve 1-3 of the second road gas 1-10 and second flowmeter 1-4, and first
Control valve 1-1 and the series connection of first flowmeter 1-2, the first control valve 1-1 is passed through the first control valve pickup wire 1-5 and is connected controller
7, first flowmeter 1-2 connects controller 7 by first flowmeter pickup wire 1-6；Second control valve 1-3 and second flowmeter
1-4 connects, and the second control valve 1-3 is passed through the second control valve pickup wire 1-7 and connected controller 7, and second flowmeter 1-4 passes through the
Two flowmeter sensor line 1-8 connect controller 7.Above-mentioned flowmeter is horizontally arranged at the front end positioned at corresponding control valve, uses
In the size of measurement gas flow, flowmeter control valve is used for adjusting gas flow size.Controller is according to the gas monitoring
Uninterrupted carries out Dynamic comparison with obtaining target gas flow value, obtains object gas by the opening degree of adjusting control valve
Flow value.
Furnace pressure control device 2 includes: is connected to the first absolute pressure meter 2-1, the second absolute pressure meter 2- on vacuum pumping hardware 2-4
2 and be connected on gas supply device 1 gas path pipe the 3rd absolute pressure meter 2-3 and vacuum pumping hardware 2-4, the first absolute pressure
Meter 2-1, the second absolute pressure meter 2-2, the 3rd absolute pressure meter 2-3 are connected respectively the first absolute pressure flowmeter sensor line on controller 7
2-5, the 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 located at the side upper end of chemical vapor deposition stove body 6, the front end of vacuum pumping hardware 2-4, the first absolute pressure meter 2-1
The pressure of monitoring vacuum pumping hardware 2-4 front end；Second absolute pressure meter 2-2 near chemical vapor deposition stove body 6, with the first absolute pressure meter
2-1 is arranged in same level, and cavity between long-pending room 5 is oozed in the second absolute pressure meter 2-2 reflection chemical vapor deposition stove body 6 and closing
Pressure；3rd absolute pressure meter 2-3 is arranged on furnace bottom air inlet 6-11 lower end, oozes the pressure in long-pending room 5 for monitoring closing.Second
Absolute pressure meter 2-2, vacuum pumping hardware 2-4 pass through the second absolute pressure flowmeter sensor line 2-6, vacuum pumping hardware pickup wire 2- respectively
8 are connected with controller 7, by the situation of change of the pressure value of the second absolute pressure meter of display on controller 7, using controller 7
The opening degree of control and regulation vacuum pumping hardware 2-4 makes the pressure stability of the second absolute pressure meter in setup pressure value.
Mixed gas is included with preheating device 3: is formed with porous graphite plate 3-3, the heating element 3-4 of pore 3-2 and preheating thermometric passes
Sensor 3-5, porous graphite plate 3-3 are layered in the framework of heating element 3-4 by the graphite locating ring 3-1 separating around plate end,
Preheating temperature transducer 3-5 is arranged between stacking porous graphite plate 3-3 space, by temperature transducer line 3-6 and heating element
Pickup wire 3-7 electrically connects controller 7.The power adjustable of heating element, the situation according to preheating temperature can be entered on the control panel
Row adjusts and controls.Porous graphite plate 3-3 is used for mixing gas and ventilation, can place multilayer, each other use graphite locating ring 3-1 every
Open, simultaneously for ensureing pre-heat effect, the pore 3-2 on adjacent porous graphite cake 3-3 should mutually stagger.Reacting gas is entered by furnace bottom
Gas port 6-11 enters mixed gas and preheating device 3, and reacting gas temperature is monitored by preheating temperature transducer 3-5, and by controlling
Device 7 is adjusted controlling, and controller 7 can process the information of preheating temperature transducer 3-5, automatically adjusts on heating element 3-4
Electrical power obtains the preheating temperature needing, till reacting gas leaves mixed gas and preheating device 3.Through overmulling gas and pre- hot charging
The gas entrance postponing is oozed long-pending by the closing that ring-shaped graphite cylinder, porous graphite liner plate, composite preform, graphite cover plate shape become
Room, air-flow passes through composite preform via big gas port and little gas port directed flow, inside composite preform
Carry out oozing long-pending.
Described depth is mixed gas and is included with air-out apparatus 4: connects firmly the airslide upper plate on mixed gas with preheating device 3 upper port
4-5 and airslide lower plate 4-1, airslide upper plate 4-5 plate body is formed with passage 4-3 and gas port 4-4, airslide lower plate 4-1
Air slot 4-2 is constituted and airslide upper plate 4-5 between.Led by gas port 4-4 entrance with the gas after preheating device 3 through overmulling gas
Air drain 4-2 carries out depth once again and mixes and disperse, finally by passage 4-3 enter closing ooze in long-pending room 5,6 be evenly distributed and
Equivalently-sized air slot 4-2.
Closing is oozed long-pending room 5 and is included: separates the porous graphite liner plate 5-2, Yi Jifang being layered in ring-shaped graphite cylinder 5-1 cylinder
It is placed in the graphite cover plate 5-6 of ring-shaped graphite cylinder 5-2 the top, the plate body of porous graphite liner plate 5-2 is formed with air guide big around center
Hole 5-5 is symmetrically uniformly distributed the little gas port 5-3 of arrangement, and composite preform 5-4 is placed on the porous that long-pending room 5 is oozed in closing
On graphite lining plate 5-2.
Chemical vapor deposition stove body 6 includes: by being formed with the heating graphite that the top graphite cover 6-2 of venthole 6-13 seals
Body 6-5, graphite heater 6-5, top graphite cover 6-2, bottom graphite cake 6-9 outer surface be respectively coated by furnace wall carbon felt 6-4,
Top carbon felt 6-1, furnace bottom carbon felt 6-10, top carbon felt 6-1, furnace bottom carbon felt 6-10 are all tightly connected with furnace wall carbon felt 6-4, top
Carbon felt 6-1 upper end is provided with graphite platen 6-8 and by the observation of graphite platen 6-8, top carbon felt 6-1 and top graphite cover 6-2
Window graphite tube 6-6 and monitoring sensor graphite tube 6-7, monitoring sensor 6-15 are arranged in the cylinder of graphite tube 6-7；Sensing
Coil 6-3 is installed between furnace wall carbon felt 6-4 and the furnace wall of chemical vapor deposition stove body 6, under chemical vapor deposition stove body 6 bottom
Fang Shunci is provided with the temperature control sensing of the furnace bottom air inlet 6-11 of high-alumina brick 6-12, furnace bottom carbon felt 6-10 and graphite cake 6-9 center
Device 6-14, temperature-control senser 6-14 electrically connect controller 7.
The operation principle of equipment is composite preform to be positioned over closing ooze long-pending interior, is heated to predetermined temperature, warp
Gas supply device flow by a certain percentage be passed through one or more reacting gas carry out mixing with preheating device through mixed gas and
Preheating, subsequently enter depth mix gas be further mixed with air-out apparatus and disperse, with after penetrate into through porous graphite liner plate
Close and ooze long-pending interior, and Stress control is carried out under certain definite value by chemical vapor infiltration by furnace pressure control device and amass.It is embodied as walking
Rapid inclusion:
(1) shove charge: composite preform 5-4 is put on the porous graphite liner plate 5-2 in chemical vapor deposition stove 6,
Install ring-shaped graphite cylinder 5-1, cover graphite cover plate 5-6, form closing and ooze long-pending room 5；
(2) vacuumize simultaneously leak check situation: open vacuum pumping hardware 2-4, chemical vapor deposition stove 6 is carried out take out very
Sky, discharges the air in chemical vapor deposition stove 6, and the pressure being evacuated to the second absolute pressure meter 2-2 is 500pa～1000pa, stops
Only vacuumize, the pressure change checking chemical vapor deposition stove 6 is to judge leakage situation；
(3) energising heats up and heats: energising intensification is heated to predetermined temperature, and is evacuated to 500pa～1000pa, in advance simultaneously
Constant temperature degree oozes the temperature-control senser 5-14 of furnace temperature thermal field and two monitoring sensor 6-15 difference in long-pending room 5 for monitoring closing
Reach predetermined temperature range and be stably defined.
(4) it is passed through reacting gas (natural gas and propane): flow by a certain percentage in the gas circuit of gas supply device 1
Each lead into natural gas and propane, flowmeter (1-2,1-4) is used for measuring the size of gas flow, and control valve (1-1,1-3) is used
In adjusting gas flow, control valve 1-1, flowmeter 1-2 and control valve 1-3, flowmeter 1-4 pass through respective pickup wire 1-5,1-
6 and 1-7,1-8 be connected with controller 7, controller 7 according to the gas flow size monitoring with obtain target gas flow value
Carry out Dynamic comparison, obtain target gas flow value by adjusting the opening degree of corresponding control valve 1-1,1-3.
(5) mixing of reacting gas (natural gas and propane) and preheating: the reacting gas after gas supply device 1 by
Furnace bottom air inlet 6-11 imports mixed gas and carries out in preheating device 3 mixing, preheats, and is configured with monitoring in mixed gas and preheating device 3
The preheating temperature transducer 3-5 of reacting gas temperature and electrical power adjustable heating element 3-4 of preheating reacting gas, preheating is surveyed
Temperature sensor 3-5 and heating element 3-4 is connected with controller 7 by temperature transducer line 3-6, heating element pickup wire 3-7, controls
Device 7 can obtain preheating temperature transducer 3-5 information, controller 7 according to obtain preheating temperature transducer 3-5 information Lai
The preheating temperature to reach needs for the electrical power of regulation heating device 3-4, heating element 3-4 is independent graphite heater.
Reacting gas carries out the mixing of short time in mixed gas and preheating device 3, after preheating, then rapidly enters adjacent
The depth being positioned above mixes gas and air-out apparatus 4, and reacting gas mixes the gas port 4-4 quilt in gas and air-out apparatus 4 by depth
The air slot 4-2 that Decentralized Pull in six is evenly distributed, mixes further, disperses in air slot 4-2 reaction gases, be then passed through
Porous graphite liner plate 5-2 infiltrates through and is placed on the composite preform 5-4 that closing is oozed in long-pending room 5, carries out chemical vapor infiltration and amasss.
Mixed gas is used for mixing gas and ventilation with the porous graphite plate 3-3 in preheating device 3, and thickness of slab is 20mm, places four layers altogether,
Height for the graphite locating ring 3-1 of positioning is 32mm, and the pore 3-2 on porous graphite plate 3-3 is φ 11mm；Depth mixes gas
With in air-out apparatus 4 passage 4-3 for φ 10mm.The width of air slot 4-2 is 10mm, highly for 10mm, on airslide 4-5
The thickness of plate is 20mm.
(6) control of furnace pressure: close the reacting gas oozing long-pending room 5 or waste gas through the venthole 6- on the graphite cover 6-2 of top
13 are discharged by vacuum pumping hardware 2-4, and furnace pressure is adjusted by furnace pressure control device 2 controlling, 2-2 in terms of the second absolute pressure
Pressure be technology controlling and process pressure.
(7) blowing out: chemical vapor infiltration amasss after reaching the scheduled time, stops being passed through reacting gas, stops vacuumizing, and stop
Electrified regulation, comes out of the stove when chemical vapor deposition stove is cooled to below 100 DEG C.
According to the present invention, component can be made to obtain homogeneous pyrolysis carbon structure, improve utilization rate and the densification speed of reacting gas
Rate, is described further below by embodiment 1.
Embodiment 1:
(1) shove charge: by 20 composite preforms (specification is 200mm × 200mm × 16mm) the horizontally mounted chemistry of 5-4
On porous graphite liner plate 5-2 in gaseous phase deposition stove 6, ring-shaped graphite cylinder 5-1 is placed on and overlays porous graphite liner plate 5-2
On, coping stone inky cap plate 5-6, on ring-shaped graphite cylinder 5-1, forms closing and oozes long-pending room 5；
The thickness of porous graphite liner plate is 30mm, and big 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 and leak check situation: chemical vapor deposition stove 6 is vacuumized, is evacuated to the second absolute pressure
The pressure of meter 2-2 is 500pa, stops vacuumizing, and checks the pressure no significant change of chemical vapor deposition stove 6；
(3) energising heats up and heats: energising intensification is heated to 1050 DEG C, and is evacuated to the second absolute pressure meter pressure 2-2 simultaneously
For 1kpa, treat that temperature-control senser 6-14 reaches and stablizes at 1050 DEG C, the temperature of other two monitoring sensor 6-15 is respectively
Stablize for 1048 DEG C, 1048 DEG C.
(4) it is passed through reacting gas (natural gas and propane): first via gas 1-9, the second road gas each lead into natural gas
With propane, gas discharge is 10l/min, and the volume ratio of natural gas/propane is 10:1, and natural gas is led to respectively with the flow of propane
Cross the first control valve 1-1 in gas supply device 1, first flowmeter 1-2 and the second control valve, second flowmeter to be adjusted
Control, to obtain required flow.
(5) mixing of reacting gas and preheating: natural gas flows into mixed gas and pre- hot charging with propane by furnace bottom air inlet 6-11
Put and carry out in 3 mixing, heat, the preheating temperature of both gaseous mixtures is by the preheating configuring monitoring temperature in mixed gas with preheating device
Temperature transducer 3-5 and electrical power adjustable heating element 3-4 adjusts control jointly, and then both gaseous mixtures are fast by pore 3-2
Speed is flowed into the mixed gas of adjacent depth and is mixed further with air-out apparatus 4, disperses, and is then passed through porous graphite liner plate 5-2 and infiltrates through
It is placed on the composite preform 5-4 that closing is oozed in long-pending room 5, carry out chemical vapor infiltration and amass.
Mixed gas is used for mixing gas and ventilation with the porous graphite plate 3-3 in preheating device 3, and thickness of slab is 20mm, places four layers altogether,
Height for the graphite locating ring 3-1 of positioning is 32mm, and the pore 3-2 on porous graphite plate 3-3 is φ 11mm；Depth mixes gas
With in air-out apparatus 4 passage 4-3 for φ 10mm.The width of air slot 4-2 is 10mm, highly for 10mm, on airslide 4-5
The thickness of plate is 20mm.
(6) control of furnace pressure: close the reacting gas oozing long-pending room or waste gas through the venthole 6-13 on the graphite cover 6-2 of top
Discharged by vacuum pumping hardware 2-4, furnace pressure is adjusted by furnace pressure control device 3 controlling, the pressure of absolute pressure meter 2 (2-2)
Power is controlled to 2.5kpa.
(7) blowing out: after chemical vapor infiltration amasss 285h, stop being passed through natural gas, propane, stop vacuumizing, and stop being energized
Heating, comes out of the stove when chemical vapor deposition stove is cooled to 90 DEG C.
By embodiment 1, the rough layer pyrolytic carbon of the final even structure obtaining, averag density reached 1.63g/cm3～
1.70g/cm3.
Claims (10)
1. a kind of carbon/carbon composite component chemical vapor infiltration amasss device, connects chemical vapor deposition stove including from bottom of furnace body
The gas supply device (1) of body (6), the furnace pressure control device (2) connecting gas supply device (1) by steam line, setting
In chemical vapor deposition stove body furnace chamber, mixed gas and air-out apparatus (4) and closing ooze long-pending room to mixed gas with the depth of preheating device (3)
(5) it is characterised in that: closing is oozed long-pending room (5) depth that is connected and is mixed gas and air-out apparatus (4), and depth is mixed under gas and air-out apparatus (4)
Side is provided with mixed gas and preheating device (3), mixed gas and the preheating device that one-level cooperation liner plate with holes controls reacting gas water conservancy diversion direction
Inside it is provided with the temperature transducer (3-5) of monitoring reacting gas preheating temperature；Gas supply device (1), furnace pressure control device (2) and
Mixed gas electrically connects controller (7) with preheating device (3)；Reacting gas temperature is monitored by temperature transducer (3-5), and by controlling
Device (7) processed is adjusted controlling, and the reacting gas of adjusted control passes through chemical gas after vacuumizing for the gas supply device (1)
Mutually deposition body of heater (6) furnace bottom air inlet (6-11) is entered mixed gas and is mixed with preheating device (3) and preheat, controller (7) root
According to the information of temperature transducer (3-5), the electrical power automatically adjusting on heating element (3-4) obtains the preheating temperature needing；Preheating
Reacting gas enters depth to be mixed gas and is further mixed with air-out apparatus (4) and disperses, and entrance is by ring-shaped graphite cylinder (5-1), many
The closing that hole graphite lining plate (5-2), composite preform (5-4), graphite cover plate (5-6) are formed oozes long-pending room (5), through porous
Graphite lining plate (5-2) infiltrates through and is placed on the composite preform (5-4) that closing is oozed in long-pending room (5), in furnace pressure control device
(2) carry out chemical vapor infiltration under Stress control and the temperature controlled definite value of temperature-control senser (6-14) to amass.
2. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amass device it is characterised in that: gas supply
Device (1) includes: is connected to first control valve (1-1) and the of gas supply device (1) gas path pipe first via gas (1-9)
Flow meters (1-2), are connected to the second control valve (1-3) on the second road gas (1-10) and second flowmeter (1-4), and first
Control valve (1-1) and first flowmeter (1-2) series connection, the first control valve (1-1) passes through the first control valve pickup wire (1-5) even
Connect controller (7), first flowmeter (1-2) connects controller (7) by first flowmeter pickup wire (1-6)；Second control
Valve (1-3) and second flowmeter (1-4) series connection, the second control valve (1-3) is passed through the second control valve pickup wire (1-7) and is connected control
Device (7) processed, second flowmeter (1-4) connects controller (7) by second flowmeter pickup wire (1-8).
3. carbon/carbon composite component chemical vapor infiltration as claimed in claim 2 amass device it is characterised in that: control valve, stream
Gauge is connected with controller by respective respective sensor line, and above-mentioned flowmeter is horizontally arranged at positioned at corresponding control valve
Front end, for measuring the size of gas flow, flowmeter control valve is used for adjusting gas flow.
4. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amass device it is characterised in that: controller root
Carry out Dynamic comparison according to the gas flow size monitoring with obtaining target gas flow value, by the unlatching journey of adjusting control valve
Degree obtains target gas flow value.
5. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amass device it is characterised in that: controling of the pressure of the oven
Device (2) includes: is connected to the first absolute pressure meter (2-1) on vacuum pumping hardware (2-4), the second absolute pressure meter (2-2) and connects
The 3rd absolute pressure meter (2-3) on gas supply device (1) gas path pipe and vacuum pumping hardware (2-4), the first absolute pressure meter
(2-1), the first absolute pressure meter that the second absolute pressure meter (2-2), the 3rd absolute pressure meter (2-3) are connected respectively on controller (7) passes
Sensor line (2-5), the second absolute pressure flowmeter sensor line (2-6), vacuum pumping hardware pickup wire (2-8) and the 3rd absolute pressure meter sensing
Device line (2-7).
6. carbon/carbon composite component chemical vapor infiltration as claimed in claim 5 amass device it is characterised in that: the first absolute pressure
Meter (2-1) is located at the side upper end of chemical vapor deposition stove body (6), the front end of vacuum pumping hardware (2-4), the first absolute pressure meter
(2-1) monitor the pressure of vacuum pumping hardware (2-4) front end；The close chemical vapor deposition stove body (6) of second absolute pressure meter (2-2),
Be arranged in same level with the first absolute pressure meter (2-1), the second absolute pressure meter (2-2) reflection chemical vapor deposition stove body (6) with
The pressure of cavity between long-pending room (5) is oozed in closing；3rd absolute pressure meter (2-3) is arranged on furnace bottom air inlet (6-11) lower end, for supervising
Survey closing and ooze the pressure in long-pending room (5).
7. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amass device it is characterised in that: mixed gas with pre-
Thermal (3) includes: is formed with porous graphite plate (3-3), heating element (3-4) and the preheating temperature transducer (3- of pore (3-2)
5) the graphite locating ring (3-1) that, porous graphite plate (3-3) passes through to separate around plate end is layered in the framework of heating element (3-4),
Preheating temperature transducer (3-5) is arranged between stacking porous graphite plate (3-3) space, by temperature transducer line (3-6) and
Heating element pickup wire (3-7) electrical connection controller (7).
8. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amass device it is characterised in that: described depth
Mixed gas is included with air-out apparatus (4): connects firmly the airslide upper plate (4-5) on mixed gas with preheating device (3) upper port and air-flow
Groove lower plate (4-1), airslide upper plate (4-5) plate body is formed with passage (4-3) and gas port (4-4), airslide lower plate (4-1)
Air slot (4-2) is constituted and airslide upper plate (4-5) between；Gas after overmulling gas and preheating device (3) is by gas port (4-
4) enter air slot (4-2) to carry out depth once again and mix and disperse, finally closing is entered by passage (4-3) and ooze in long-pending room (5).
9. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amass device it is characterised in that: closing ooze long-pending
Room (5) includes: separates the porous graphite liner plate (5-2) being layered in ring-shaped graphite cylinder (5-1) cylinder, and is positioned over annular stone
The graphite cover plate (5-6) of ink cylinder (5-2) the top, the plate body of porous graphite liner plate (5-2) is formed with around center big gas port (5-
5) symmetrically it is uniformly distributed the little gas port (5-3) of arrangement, composite preform (5-4) is placed on closing and oozes long-pending room (5)
On porous graphite liner plate (5-2).
10. carbon/carbon composite component chemical vapor infiltration as claimed in claim 1 amass device it is characterised in that: chemical gaseous phase
Deposition body of heater (6) includes: by being formed with the graphite heater (6-5) that the top graphite cover (6-2) of venthole (6-13) seals, bag
Overlay on the furnace wall carbon felt (6-4) that graphite heater (6-5) outer surface sealed by top carbon felt (6-1), in top carbon felt (6-1)
End is provided with graphite platen (6-8) and by the observation window of graphite platen (6-8), top carbon felt (6-1) and top graphite cover (6-2)
Graphite tube (6-6) and monitoring sensor, with graphite tube (6-7), monitor the cylinder that sensor (6-15) is arranged on graphite tube (6-7)
Interior；High-alumina brick (6-12) that induction coil (6-3) is sequentially connected by chemical vapor deposition stove body (6) bottom part down, furnace bottom carbon
The furnace bottom air inlet (6-11) electrical connection temperature-control senser (6-14) at felt (6-10) and graphite cake (6-9) center.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410675591.2A CN104498891B (en) | 2014-11-23 | 2014-11-23 | Carbon/carbon composite component chemical vapor infiltration device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410675591.2A CN104498891B (en) | 2014-11-23 | 2014-11-23 | Carbon/carbon composite component chemical vapor infiltration device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104498891A CN104498891A (en) | 2015-04-08 |
| CN104498891B true CN104498891B (en) | 2017-01-25 |
Family
ID=52940341
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410675591.2A Active CN104498891B (en) | 2014-11-23 | 2014-11-23 | Carbon/carbon composite component chemical vapor infiltration device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104498891B (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420686B (en) * | 2015-12-31 | 2019-06-25 | 清远先导材料有限公司 | A kind of chemical vapor deposition stove graphite deposits device |
| CN107099782A (en) * | 2016-02-23 | 2017-08-29 | 常州国成新材料科技有限公司 | A kind of chemical vapor deposition unit for preparing the thin-film materials such as graphene, hexagonal boron nitride |
| CN108070848A (en) * | 2016-11-11 | 2018-05-25 | 优材科技有限公司 | Heater module, film deposition apparatus and method |
| CN107058977A (en) * | 2017-04-17 | 2017-08-18 | 湖南红太阳光电科技有限公司 | A kind of PECVD film plating process and device |
| CN108558427B (en) * | 2018-05-22 | 2020-11-13 | 中南大学 | Method for batch preparation of carbon/carbon composite material flat plate with uniform density by using confined reactor |
| 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 |
| CN113106428B (en) * | 2021-04-07 | 2022-07-26 | 锦州同创真空冶金科技有限公司 | Vacuum induction chemical vapor deposition furnace |
| 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 |
| CN115094402B (en) * | 2022-06-24 | 2023-04-11 | 清华大学 | Vertical double-temperature-zone-double-channel chemical vapor deposition equipment |
| CN115636685B (en) * | 2022-10-27 | 2023-08-15 | 上饶中昱新材料科技有限公司 | Method and system for preparing large cylindrical carbon-carbon thermal field material in short period through multiple material columns of CVI (chemical vapor infiltration) system |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2881145B1 (en) * | 2005-01-24 | 2007-11-23 | Snecma Propulsion Solide Sa | METHOD OF GAS PHASE CHEMICAL INFILTRATION FOR THE DENSIFICATION OF POROUS SUBSTRATES WITH PYROLYTIC CARBON |
| CN201144282Y (en) * | 2007-09-14 | 2008-11-05 | 北京航空航天大学 | Temperature gradient direction flow vapor deposition furnace for preparing charcoal/charcoal member |
| CN101215182B (en) * | 2008-01-09 | 2010-11-17 | 西安航天复合材料研究所 | Device and method for preparing carbon/carbon composite material with gradient distribution density |
| CN203530428U (en) * | 2013-10-29 | 2014-04-09 | 成都润封电碳有限公司 | Vapor deposition furnace for coating silicon carbide on large-scale graphite sleeve |
-
2014
- 2014-11-23 CN CN201410675591.2A patent/CN104498891B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104498891A (en) | 2015-04-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104498891B (en) | Carbon/carbon composite component chemical vapor infiltration device | |
| CN1298888C (en) | Apparatus for use with CVI/CVD processes | |
| CN104297648B (en) | Temperature and flow speed control device used for transformer oil insulation heat ageing test and test method thereof | |
| CN101712026B (en) | Baking oven for adhesive coated foil | |
| CN103193498A (en) | Narrow flow induction coupling chemical vapor deposition (CVD) densification method for rapidly preparing carbon/carbon composite material crucible | |
| CN104596235A (en) | Combined type microwave sintering furnace | |
| CN107400875A (en) | A kind of hot-filament chemical vapor deposition equipment | |
| CN203461974U (en) | Homogenization fast device of CVI (Chemical Vapor Infiltration) compact carbon/carbon crucible | |
| CN108796473A (en) | A kind of thermal decomposition preparation method of film | |
| CN107741468A (en) | A kind of catalyst test apparatus of magneto-optic heat collaboration | |
| CN100546945C (en) | The rapid chemical liquid-phase vaporization osmose process prepares the technology of charcoal/charcoal component | |
| CN112423418B (en) | Fluid material microwave heating device and intelligent control method thereof | |
| CN102618851B (en) | Tool for compacting thick-walled hollow carbon/carbon (C/C) composite product | |
| CN110978569B (en) | Gas flow field structure in plate CVI process | |
| CN104155227A (en) | Oil-gas permeability testing apparatus based on hollow fibrous membrane and oil-gas permeability testing method | |
| CN101671188A (en) | Gas flow control method of rapid directional infiltration for high-performance carbon-based composite material | |
| CN206184050U (en) | Bubble system is arranged to substrate glue | |
| CN216831522U (en) | Evaporate and press aerated concrete wall processing with evaporating device | |
| CN105547977A (en) | A sulfate test chamber with a high-temperature resistant layer | |
| CN104926349A (en) | Method and depositing furnace for rapidly depositing and preparing C/C composite material by direct heating method | |
| CN201154987Y (en) | Novel liquid phase vaporization densification device for preparing C/C component | |
| CN108444282A (en) | The kiln and de-waxing method of semi-finished product de-waxing are noted for ceramics injection | |
| CN203857793U (en) | Chamber electric furnace | |
| CN203018067U (en) | Stratification heat type reaction kettle | |
| CN111235548A (en) | Fiber reinforced composite material deposition furnace based on CVD/CVI (chemical vapor deposition/chemical vapor deposition) double process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information |
Inventor after: Zhang You Inventor after: Xu Chun Inventor after: Ye Yongsong Inventor after: Peng Zhongya Inventor after: Yang Dongling Inventor after: Liu Junling Inventor after: Zhang Liangcheng Inventor after: Gu Wenxue Inventor before: Xiang Qiao Inventor before: Peng Zhongya Inventor before: Ye Yongsong Inventor before: Yang Dongling Inventor before: Liu Junling Inventor before: Zhang Liangcheng |
|
| COR | Change of bibliographic data | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |